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

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

data_ba_jb15
_database_code_depnum_ccdc_archive 'CCDC 1440950'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;
_audit_creation_date             2015-12-03

_audit_block_code                ba_jb15
_audit_block_refno               2376
_audit_block_usercomment         jb228


_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C24 H27 Cl2 N2 P Ti'
_chemical_formula_sum            'C24 H27 Cl2 N2 P Ti'
_chemical_properties_physical    moisture-sensitive
_chemical_formula_weight         493.24
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            black
_diffrn_ambient_temperature      100(1)
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'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14

_chemical_absolute_configuration .

_space_group_name_Hall           '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.314(3)
_cell_length_b                   19.255(8)
_cell_length_c                   15.270(7)
_cell_angle_alpha                90
_cell_angle_beta                 104.617(8)
_cell_angle_gamma                90
_cell_volume                     2365.3(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8162
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.32
_cell_measurement_theta_min      2.53
_shelx_estimated_absorpt_T_max   0.906
_shelx_estimated_absorpt_T_min   0.762
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6929

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.150
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60410
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.451
_diffrn_reflns_theta_min         2.115
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7047
_reflns_number_total             8160
_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 (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        
'SAINT V8.34A (Bruker AXS, 1997-2013),SADABS-2014_4 (Sheldrick and Bruker AXS, 1997-2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         8160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0289
_refine_ls_restrained_S_all      1.059
_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)+(0.0344P)²+1.2840P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0761
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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 0.80195(2) 0.64206(2) 0.36735(2) 0.00850(4) Uani 1 1 d . . . . .
Cl1 Cl 0.53373(3) 0.59604(2) 0.33660(2) 0.01634(6) Uani 1 1 d . . . . .
Cl2 Cl 0.80468(4) 0.64996(2) 0.52113(2) 0.01611(6) Uani 1 1 d . . . . .
P P 1.10423(3) 0.67846(2) 0.42532(2) 0.01044(6) Uani 1 1 d . . . . .
N1 N 0.89692(11) 0.56710(5) 0.31513(6) 0.01075(16) Uani 1 1 d . . . . .
N2 N 0.77700(11) 0.72412(5) 0.29395(6) 0.01047(16) Uani 1 1 d . . . . .
C1 C 1.23616(14) 0.60386(6) 0.46915(8) 0.0148(2) Uani 1 1 d . . . . .
H1A H 1.348(2) 0.6168(9) 0.4743(11) 0.018 Uiso 1 1 d R . . . .
H1B H 1.2210(19) 0.5956(8) 0.5290(11) 0.018 Uiso 1 1 d R . . . .
C2 C 1.18525(14) 0.53902(6) 0.41016(8) 0.0146(2) Uani 1 1 d . . . . .
H2A H 1.220(2) 0.5433(8) 0.3542(11) 0.018 Uiso 1 1 d R . . . .
H2B H 1.246(2) 0.4992(9) 0.4417(11) 0.018 Uiso 1 1 d R . . . .
C3 C 0.99809(13) 0.52400(6) 0.38824(7) 0.01282(19) Uani 1 1 d . . . . .
H3A H 0.9718(19) 0.4764(8) 0.3736(11) 0.015 Uiso 1 1 d R . . . .
H3B H 0.9580(19) 0.5335(8) 0.4422(11) 0.015 Uiso 1 1 d R . . . .
C4 C 0.86635(13) 0.54154(5) 0.22643(7) 0.01098(18) Uani 1 1 d . . . . .
C5 C 0.96413(15) 0.48961(6) 0.20105(8) 0.0160(2) Uani 1 1 d . . . . .
H5 H 1.055(2) 0.4702(9) 0.2463(11) 0.019 Uiso 1 1 d R . . . .
C6 C 0.92763(17) 0.46596(6) 0.11226(9) 0.0204(2) Uani 1 1 d . . . . .
H6 H 0.999(2) 0.4298(9) 0.0989(12) 0.025 Uiso 1 1 d R . . . .
C7 C 0.79442(17) 0.49307(7) 0.04716(8) 0.0208(2) Uani 1 1 d . . . . .
H7 H 0.770(2) 0.4759(9) -0.0128(12) 0.025 Uiso 1 1 d R . . . .
C8 C 0.69667(15) 0.54434(6) 0.07175(8) 0.0174(2) Uani 1 1 d . . . . .
H8 H 0.609(2) 0.5631(9) 0.0283(11) 0.021 Uiso 1 1 d R . . . .
C9 C 0.73126(14) 0.56817(6) 0.16024(7) 0.01316(19) Uani 1 1 d . . . . .
H9 H 0.6665(19) 0.6009(8) 0.1766(11) 0.016 Uiso 1 1 d R . . . .
C10 C 1.17353(13) 0.70884(6) 0.32716(8) 0.01390(19) Uani 1 1 d . . . . .
H10A H 1.282(2) 0.7286(8) 0.3497(11) 0.017 Uiso 1 1 d R . . . .
H10B H 1.185(2) 0.6686(9) 0.2941(11) 0.017 Uiso 1 1 d R . . . .
C11 C 1.05212(14) 0.75903(6) 0.26637(8) 0.01355(19) Uani 1 1 d . . . . .
H11A H 1.0973(19) 0.7726(8) 0.2162(11) 0.016 Uiso 1 1 d R . . . .
H11B H 1.040(2) 0.8014(8) 0.2994(11) 0.016 Uiso 1 1 d R . . . .
C12 C 0.88128(13) 0.72577(6) 0.22816(7) 0.01156(18) Uani 1 1 d . . . . .
H12A H 0.8209(19) 0.7491(8) 0.1743(10) 0.014 Uiso 1 1 d R . . . .
H12B H 0.8961(19) 0.6778(8) 0.2097(10) 0.014 Uiso 1 1 d R . . . .
C13 C 0.68841(13) 0.78547(5) 0.30201(7) 0.01158(18) Uani 1 1 d . . . . .
C14 C 0.59208(14) 0.78724(6) 0.36551(8) 0.0150(2) Uani 1 1 d . . . . .
H14 H 0.590(2) 0.7485(9) 0.4029(11) 0.018 Uiso 1 1 d R . . . .
C15 C 0.49606(15) 0.84488(7) 0.37267(9) 0.0197(2) Uani 1 1 d . . . . .
H15 H 0.434(2) 0.8463(9) 0.4138(12) 0.024 Uiso 1 1 d R . . . .
C16 C 0.49321(17) 0.90231(7) 0.31713(10) 0.0246(3) Uani 1 1 d . . . . .
H16 H 0.424(2) 0.9414(10) 0.3218(12) 0.030 Uiso 1 1 d R . . . .
C17 C 0.58993(17) 0.90159(7) 0.25525(10) 0.0237(3) Uani 1 1 d . . . . .
H17 H 0.591(2) 0.9398(10) 0.2153(12) 0.028 Uiso 1 1 d R . . . .
C18 C 0.68784(15) 0.84421(6) 0.24746(9) 0.0179(2) Uani 1 1 d . . . . .
H18 H 0.749(2) 0.8448(9) 0.2046(12) 0.021 Uiso 1 1 d R . . . .
C19 C 1.16399(13) 0.74647(6) 0.50906(7) 0.01261(19) Uani 1 1 d . . . . .
C20 C 1.04960(14) 0.79888(6) 0.51278(8) 0.01431(19) Uani 1 1 d . . . . .
H20 H 0.938(2) 0.7962(8) 0.4720(11) 0.017 Uiso 1 1 d R . . . .
C21 C 1.09435(15) 0.85399(6) 0.57293(8) 0.0154(2) Uani 1 1 d . . . . .
H21 H 1.017(2) 0.8874(9) 0.5748(11) 0.018 Uiso 1 1 d R . . . .
C22 C 1.25300(16) 0.85674(6) 0.63039(8) 0.0170(2) Uani 1 1 d . . . . .
H22 H 1.282(2) 0.8925(9) 0.6707(11) 0.020 Uiso 1 1 d R . . . .
C23 C 1.36564(15) 0.80380(7) 0.62910(8) 0.0189(2) Uani 1 1 d . . . . .
H23 H 1.472(2) 0.8035(9) 0.6710(11) 0.023 Uiso 1 1 d R . . . .
C24 C 1.32238(14) 0.74906(6) 0.56829(8) 0.0170(2) Uani 1 1 d . . . . .
H24 H 1.402(2) 0.7140(9) 0.5653(11) 0.020 Uiso 1 1 d 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 Cl1 2.3345(9) . ?
Ti Cl2 2.3476(11) . ?
Ti P 2.5431(10) . ?
Ti N1 1.9131(10) . ?
Ti N2 1.9181(11) . ?
P C1 1.8286(12) . ?
P C10 1.8322(13) . ?
P C19 1.8100(12) . ?
N1 C3 1.4727(14) . ?
N1 C4 1.4027(15) . ?
N2 C12 1.4836(14) . ?
N2 C13 1.4137(14) . ?
C1 H1A 0.943(17) . ?
C1 H1B 0.966(16) . ?
C1 C2 1.5352(17) . ?
C2 H2A 0.972(16) . ?
C2 H2B 0.977(16) . ?
C2 C3 1.5342(17) . ?
C3 H3A 0.956(16) . ?
C3 H3B 0.980(16) . ?
C4 C5 1.4035(16) . ?
C4 C9 1.4047(15) . ?
C5 H5 0.963(16) . ?
C5 C6 1.3893(18) . ?
C6 H6 0.966(18) . ?
C6 C7 1.3897(19) . ?
C7 H7 0.946(18) . ?
C7 C8 1.3892(18) . ?
C8 H8 0.928(17) . ?
C8 C9 1.3867(17) . ?
C9 H9 0.905(16) . ?
C10 H10A 0.961(16) . ?
C10 H10B 0.942(17) . ?
C10 C11 1.5302(16) . ?
C11 H11A 0.970(16) . ?
C11 H11B 0.978(16) . ?
C11 C12 1.5328(16) . ?
C12 H12A 0.960(15) . ?
C12 H12B 0.983(16) . ?
C13 C14 1.4052(16) . ?
C13 C18 1.4041(16) . ?
C14 H14 0.941(17) . ?
C14 C15 1.3875(17) . ?
C15 H15 0.907(18) . ?
C15 C16 1.390(2) . ?
C16 H16 0.961(19) . ?
C16 C17 1.387(2) . ?
C17 H17 0.956(18) . ?
C17 C18 1.3951(17) . ?
C18 H18 0.926(18) . ?
C19 C20 1.3977(16) . ?
C19 C24 1.3976(16) . ?
C20 H20 0.982(16) . ?
C20 C21 1.3912(16) . ?
C21 H21 0.915(17) . ?
C21 C22 1.3886(17) . ?
C22 H22 0.914(17) . ?
C22 C23 1.3876(19) . ?
C23 H23 0.949(17) . ?
C23 C24 1.3907(17) . ?
C24 H24 0.954(17) . ?

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
Cl1 Ti Cl2 89.623(16) . . ?
Cl1 Ti P 169.896(14) . . ?
Cl2 Ti P 82.803(17) . . ?
N1 Ti Cl1 95.95(4) . . ?
N1 Ti Cl2 124.40(3) . . ?
N1 Ti P 82.96(4) . . ?
N1 Ti N2 111.90(5) . . ?
N2 Ti Cl1 103.78(3) . . ?
N2 Ti Cl2 120.23(3) . . ?
N2 Ti P 85.87(3) . . ?
C1 P Ti 111.08(5) . . ?
C1 P C10 105.48(6) . . ?
C10 P Ti 106.88(4) . . ?
C19 P Ti 121.08(4) . . ?
C19 P C1 106.10(6) . . ?
C19 P C10 105.07(6) . . ?
C3 N1 Ti 109.02(7) . . ?
C4 N1 Ti 132.37(7) . . ?
C4 N1 C3 117.64(9) . . ?
C12 N2 Ti 114.70(7) . . ?
C13 N2 Ti 128.27(8) . . ?
C13 N2 C12 116.57(9) . . ?
P C1 H1A 108.0(10) . . ?
P C1 H1B 105.4(10) . . ?
H1A C1 H1B 108.9(13) . . ?
C2 C1 P 111.90(8) . . ?
C2 C1 H1A 112.5(10) . . ?
C2 C1 H1B 109.8(10) . . ?
C1 C2 H2A 110.4(10) . . ?
C1 C2 H2B 108.5(9) . . ?
H2A C2 H2B 105.5(13) . . ?
C3 C2 C1 113.30(9) . . ?
C3 C2 H2A 109.5(9) . . ?
C3 C2 H2B 109.4(10) . . ?
N1 C3 C2 114.39(9) . . ?
N1 C3 H3A 108.1(9) . . ?
N1 C3 H3B 106.4(9) . . ?
C2 C3 H3A 113.0(9) . . ?
C2 C3 H3B 108.8(9) . . ?
H3A C3 H3B 105.5(13) . . ?
N1 C4 C5 122.70(10) . . ?
N1 C4 C9 118.94(10) . . ?
C5 C4 C9 118.36(10) . . ?
C4 C5 H5 118.9(10) . . ?
C6 C5 C4 120.26(11) . . ?
C6 C5 H5 120.8(10) . . ?
C5 C6 H6 116.5(10) . . ?
C5 C6 C7 120.89(11) . . ?
C7 C6 H6 122.6(10) . . ?
C6 C7 H7 119.8(11) . . ?
C8 C7 C6 119.24(11) . . ?
C8 C7 H7 120.9(11) . . ?
C7 C8 H8 119.6(10) . . ?
C9 C8 C7 120.46(11) . . ?
C9 C8 H8 119.9(10) . . ?
C4 C9 H9 118.6(10) . . ?
C8 C9 C4 120.79(11) . . ?
C8 C9 H9 120.6(10) . . ?
P C10 H10A 107.1(9) . . ?
P C10 H10B 105.7(10) . . ?
H10A C10 H10B 107.9(14) . . ?
C11 C10 P 113.73(8) . . ?
C11 C10 H10A 112.6(10) . . ?
C11 C10 H10B 109.4(10) . . ?
C10 C11 H11A 108.8(9) . . ?
C10 C11 H11B 110.7(9) . . ?
C10 C11 C12 111.90(9) . . ?
H11A C11 H11B 107.1(13) . . ?
C12 C11 H11A 108.6(9) . . ?
C12 C11 H11B 109.7(9) . . ?
N2 C12 C11 113.26(9) . . ?
N2 C12 H12A 108.7(9) . . ?
N2 C12 H12B 108.1(9) . . ?
C11 C12 H12A 111.4(9) . . ?
C11 C12 H12B 109.3(9) . . ?
H12A C12 H12B 105.7(13) . . ?
C14 C13 N2 118.72(10) . . ?
C18 C13 N2 123.04(10) . . ?
C18 C13 C14 118.21(10) . . ?
C13 C14 H14 119.9(10) . . ?
C15 C14 C13 120.88(11) . . ?
C15 C14 H14 119.2(10) . . ?
C14 C15 H15 121.0(11) . . ?
C14 C15 C16 120.65(12) . . ?
C16 C15 H15 118.3(11) . . ?
C15 C16 H16 119.8(11) . . ?
C17 C16 C15 118.96(12) . . ?
C17 C16 H16 121.2(11) . . ?
C16 C17 H17 121.7(11) . . ?
C16 C17 C18 121.15(12) . . ?
C18 C17 H17 117.1(11) . . ?
C13 C18 H18 120.6(11) . . ?
C17 C18 C13 120.13(12) . . ?
C17 C18 H18 119.2(11) . . ?
C20 C19 P 118.87(8) . . ?
C20 C19 C24 119.18(11) . . ?
C24 C19 P 121.93(9) . . ?
C19 C20 H20 118.8(10) . . ?
C21 C20 C19 120.41(11) . . ?
C21 C20 H20 120.8(9) . . ?
C20 C21 H21 118.9(10) . . ?
C22 C21 C20 119.95(11) . . ?
C22 C21 H21 121.1(10) . . ?
C21 C22 H22 119.9(11) . . ?
C23 C22 C21 119.99(11) . . ?
C23 C22 H22 120.1(11) . . ?
C22 C23 H23 120.6(11) . . ?
C22 C23 C24 120.30(11) . . ?
C24 C23 H23 119.1(11) . . ?
C19 C24 H24 119.7(10) . . ?
C23 C24 C19 120.12(11) . . ?
C23 C24 H24 120.1(10) . . ?

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
Ti P C1 C2 39.87(9) . . . . ?
Ti P C10 C11 47.08(9) . . . . ?
Ti P C19 C20 -28.54(11) . . . . ?
Ti P C19 C24 153.23(8) . . . . ?
Ti N1 C3 C2 -99.01(9) . . . . ?
Ti N1 C4 C5 173.10(8) . . . . ?
Ti N1 C4 C9 -7.72(15) . . . . ?
Ti N2 C12 C11 -90.25(10) . . . . ?
Ti N2 C13 C14 -6.27(14) . . . . ?
Ti N2 C13 C18 175.79(9) . . . . ?
P C1 C2 C3 -48.83(12) . . . . ?
P C10 C11 C12 -60.00(11) . . . . ?
P C19 C20 C21 -176.48(9) . . . . ?
P C19 C24 C23 177.29(9) . . . . ?
N1 C4 C5 C6 179.67(11) . . . . ?
N1 C4 C9 C8 179.99(10) . . . . ?
N2 C13 C14 C15 -176.60(10) . . . . ?
N2 C13 C18 C17 176.21(11) . . . . ?
C1 P C10 C11 165.37(8) . . . . ?
C1 P C19 C20 -156.21(9) . . . . ?
C1 P C19 C24 25.56(11) . . . . ?
C1 C2 C3 N1 79.21(12) . . . . ?
C3 N1 C4 C5 -19.55(15) . . . . ?
C3 N1 C4 C9 159.63(10) . . . . ?
C4 N1 C3 C2 90.85(12) . . . . ?
C4 C5 C6 C7 0.00(19) . . . . ?
C5 C4 C9 C8 -0.80(16) . . . . ?
C5 C6 C7 C8 -0.19(19) . . . . ?
C6 C7 C8 C9 -0.12(19) . . . . ?
C7 C8 C9 C4 0.62(18) . . . . ?
C9 C4 C5 C6 0.48(17) . . . . ?
C10 P C1 C2 -75.57(10) . . . . ?
C10 P C19 C20 92.36(10) . . . . ?
C10 P C19 C24 -85.87(11) . . . . ?
C10 C11 C12 N2 78.98(12) . . . . ?
C12 N2 C13 C14 -177.99(9) . . . . ?
C12 N2 C13 C18 4.07(15) . . . . ?
C13 N2 C12 C11 82.60(11) . . . . ?
C13 C14 C15 C16 -0.08(19) . . . . ?
C14 C13 C18 C17 -1.74(18) . . . . ?
C14 C15 C16 C17 -1.0(2) . . . . ?
C15 C16 C17 C18 0.7(2) . . . . ?
C16 C17 C18 C13 0.7(2) . . . . ?
C18 C13 C14 C15 1.44(17) . . . . ?
C19 P C1 C2 173.28(8) . . . . ?
C19 P C10 C11 -82.75(9) . . . . ?
C19 C20 C21 C22 -0.69(17) . . . . ?
C20 C19 C24 C23 -0.93(18) . . . . ?
C20 C21 C22 C23 -1.32(18) . . . . ?
C21 C22 C23 C24 2.19(19) . . . . ?
C22 C23 C24 C19 -1.06(19) . . . . ?
C24 C19 C20 C21 1.80(17) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            CCD-PXL-KAF2
####################################################################### 
# 
# 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_ba_tk9
_database_code_depnum_ccdc_archive 'CCDC 1440951'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;
_audit_creation_date             2015-12-03

_audit_block_code                ba_tk9
_audit_block_refno               2475
_audit_block_usercomment         NPNZrCl2


_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C24 H27 Cl2 N2 P Zr, C H2 Cl2'
_chemical_formula_sum            'C25 H29 Cl4 N2 P Zr'
_chemical_properties_physical    moisture-sensitive
_chemical_formula_weight         621.49
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_diffrn_ambient_temperature      100(1)
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'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2

_chemical_absolute_configuration .

_space_group_name_Hall           '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.582(3)
_cell_length_b                   11.757(5)
_cell_length_c                   14.513(5)
_cell_angle_alpha                66.612(7)
_cell_angle_beta                 84.723(8)
_cell_angle_gamma                75.566(12)
_cell_volume                     1301.6(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8172
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.29
_cell_measurement_theta_min      2.45
_shelx_estimated_absorpt_T_max   0.839
_shelx_estimated_absorpt_T_min   0.771
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6575

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33951
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.529
_diffrn_reflns_theta_min         1.941
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8017
_reflns_number_total             8800
_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 (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        
'SAINT V8.34A (Bruker AXS, 1997-2013),SADABS-2014_5 (Sheldrick and Bruker AXS, 1997-2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         8800
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0225
_refine_ls_restrained_S_all      1.044
_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)+(0.0266P)²+0.6374P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0585
_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:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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 0.42942(2) 0.80470(2) 0.32534(2) 0.00921(3) Uani 1 1 d . . . . .
Cl1 Cl 0.71459(3) 0.70640(3) 0.31315(2) 0.01631(6) Uani 1 1 d . . . . .
Cl2 Cl 0.46714(4) 0.91271(3) 0.42877(2) 0.01828(6) Uani 1 1 d . . . . .
P P 0.10416(3) 0.89239(3) 0.34189(2) 0.01013(5) Uani 1 1 d . . . . .
N1 N 0.35176(11) 0.63868(9) 0.38456(7) 0.01142(16) Uani 1 1 d . . . . .
N2 N 0.37575(11) 0.91358(9) 0.17541(7) 0.01192(17) Uani 1 1 d . . . . .
C1 C 0.01481(13) 0.79107(11) 0.45429(8) 0.01322(19) Uani 1 1 d . . . . .
H1A H 0.0236 0.8170 0.5104 0.016 Uiso 1 1 calc R . . . .
H1B H -0.1009 0.8041 0.4415 0.016 Uiso 1 1 calc R . . . .
C2 C 0.09645(13) 0.64887(11) 0.48533(9) 0.0137(2) Uani 1 1 d . . . . .
H2A H 0.0605 0.6014 0.5537 0.016 Uiso 1 1 calc R . . . .
H2B H 0.0601 0.6173 0.4391 0.016 Uiso 1 1 calc R . . . .
C3 C 0.28105(13) 0.61983(11) 0.48480(8) 0.01242(19) Uani 1 1 d . . . . .
H3A H 0.3165 0.6754 0.5110 0.015 Uiso 1 1 calc R . . . .
H3B H 0.3231 0.5304 0.5309 0.015 Uiso 1 1 calc R . . . .
C4 C 0.01637(13) 0.87442(11) 0.23930(8) 0.01280(19) Uani 1 1 d . . . . .
H4A H 0.0353 0.7825 0.2533 0.015 Uiso 1 1 calc R . . . .
H4B H -0.1014 0.9090 0.2379 0.015 Uiso 1 1 calc R . . . .
C5 C 0.08408(13) 0.94124(11) 0.13571(8) 0.01295(19) Uani 1 1 d . . . . .
H5A H 0.0718 1.0321 0.1235 0.016 Uiso 1 1 calc R . . . .
H5B H 0.0201 0.9377 0.0839 0.016 Uiso 1 1 calc R . . . .
C6 C 0.26193(13) 0.88232(11) 0.12415(9) 0.01334(19) Uani 1 1 d . . . . .
H6A H 0.2779 0.7885 0.1507 0.016 Uiso 1 1 calc R . . . .
H6B H 0.2878 0.9116 0.0517 0.016 Uiso 1 1 calc R . . . .
C7 C 0.00657(13) 1.05516(11) 0.32531(8) 0.01221(19) Uani 1 1 d . . . . .
C8 C 0.08658(14) 1.15208(11) 0.27299(9) 0.0154(2) Uani 1 1 d . . . . .
H8 H 0.1945 1.1311 0.2523 0.018 Uiso 1 1 calc R . . . .
C9 C 0.00924(15) 1.27915(11) 0.25098(9) 0.0170(2) Uani 1 1 d . . . . .
H9 H 0.0640 1.3446 0.2147 0.020 Uiso 1 1 calc R . . . .
C10 C -0.14809(15) 1.31029(12) 0.28215(9) 0.0176(2) Uani 1 1 d . . . . .
H10 H -0.2012 1.3970 0.2667 0.021 Uiso 1 1 calc R . . . .
C11 C -0.22752(14) 1.21413(12) 0.33606(9) 0.0173(2) Uani 1 1 d . . . . .
H11 H -0.3342 1.2354 0.3585 0.021 Uiso 1 1 calc R . . . .
C12 C -0.15162(14) 1.08718(12) 0.35725(9) 0.0153(2) Uani 1 1 d . . . . .
H12 H -0.2069 1.0221 0.3934 0.018 Uiso 1 1 calc R . . . .
C13 C 0.35951(13) 0.54293(10) 0.34834(8) 0.01131(18) Uani 1 1 d . . . . .
C14 C 0.29356(13) 0.43638(11) 0.39930(8) 0.01332(19) Uani 1 1 d . . . . .
H14 H 0.2425 0.4260 0.4621 0.016 Uiso 1 1 calc R . . . .
C15 C 0.30267(14) 0.34604(11) 0.35838(9) 0.0156(2) Uani 1 1 d . . . . .
H15 H 0.2577 0.2745 0.3938 0.019 Uiso 1 1 calc R . . . .
C16 C 0.37638(14) 0.35869(12) 0.26664(9) 0.0164(2) Uani 1 1 d . . . . .
H16 H 0.3792 0.2980 0.2383 0.020 Uiso 1 1 calc R . . . .
C17 C 0.44603(14) 0.46199(11) 0.21704(9) 0.0152(2) Uani 1 1 d . . . . .
H17 H 0.4988 0.4708 0.1549 0.018 Uiso 1 1 calc R . . . .
C18 C 0.43916(13) 0.55200(11) 0.25731(9) 0.0135(2) Uani 1 1 d . . . . .
H18 H 0.4890 0.6210 0.2229 0.016 Uiso 1 1 calc R . . . .
C19 C 0.42067(13) 1.02987(10) 0.12405(8) 0.01172(19) Uani 1 1 d . . . . .
C20 C 0.54428(14) 1.05558(12) 0.16508(9) 0.0156(2) Uani 1 1 d . . . . .
H20 H 0.5989 0.9921 0.2241 0.019 Uiso 1 1 calc R . . . .
C21 C 0.58780(15) 1.17130(12) 0.12112(9) 0.0169(2) Uani 1 1 d . . . . .
H21 H 0.6695 1.1870 0.1513 0.020 Uiso 1 1 calc R . . . .
C22 C 0.51312(15) 1.26471(11) 0.03321(10) 0.0176(2) Uani 1 1 d . . . . .
H22 H 0.5421 1.3444 0.0034 0.021 Uiso 1 1 calc R . . . .
C23 C 0.39526(14) 1.23912(11) -0.01008(9) 0.0170(2) Uani 1 1 d . . . . .
H23 H 0.3456 1.3014 -0.0712 0.020 Uiso 1 1 calc R . . . .
C24 C 0.34826(13) 1.12406(11) 0.03415(9) 0.0138(2) Uani 1 1 d . . . . .
H24 H 0.2667 1.1092 0.0033 0.017 Uiso 1 1 calc R . . . .
Cl11 Cl 0.20028(4) 0.52344(3) 0.00260(2) 0.02117(6) Uani 1 1 d . . . . .
Cl12 Cl 0.00334(4) 0.64213(3) 0.13082(3) 0.02426(7) Uani 1 1 d . . . . .
C25 C 0.07071(16) 0.66379(13) 0.00781(10) 0.0223(2) Uani 1 1 d . . . . .
H25A H 0.1284 0.7334 -0.0172 0.027 Uiso 1 1 calc R . . . .
H25B H -0.0234 0.6894 -0.0367 0.027 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
Zr Cl1 2.4555(9) . ?
Zr Cl2 2.4038(7) . ?
Zr P 2.7480(11) . ?
Zr N1 2.0504(12) . ?
Zr N2 2.0650(12) . ?
P C1 1.8305(12) . ?
P C4 1.8342(12) . ?
P C7 1.8149(14) . ?
N1 C3 1.4772(15) . ?
N1 C13 1.4052(15) . ?
N2 C6 1.4740(15) . ?
N2 C19 1.4052(15) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.5379(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.5353(17) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.5312(16) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.5349(17) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.3978(16) . ?
C7 C12 1.4028(16) . ?
C8 H8 0.9500 . ?
C8 C9 1.3929(17) . ?
C9 H9 0.9500 . ?
C9 C10 1.3909(18) . ?
C10 H10 0.9500 . ?
C10 C11 1.3924(19) . ?
C11 H11 0.9500 . ?
C11 C12 1.3908(18) . ?
C12 H12 0.9500 . ?
C13 C14 1.4062(16) . ?
C13 C18 1.4080(16) . ?
C14 H14 0.9500 . ?
C14 C15 1.3921(17) . ?
C15 H15 0.9500 . ?
C15 C16 1.3892(18) . ?
C16 H16 0.9500 . ?
C16 C17 1.3926(17) . ?
C17 H17 0.9500 . ?
C17 C18 1.3850(17) . ?
C18 H18 0.9500 . ?
C19 C20 1.4108(16) . ?
C19 C24 1.4050(16) . ?
C20 H20 0.9500 . ?
C20 C21 1.3849(17) . ?
C21 H21 0.9500 . ?
C21 C22 1.3898(18) . ?
C22 H22 0.9500 . ?
C22 C23 1.3883(19) . ?
C23 H23 0.9500 . ?
C23 C24 1.3927(17) . ?
C24 H24 0.9500 . ?
Cl11 C25 1.7703(15) . ?
Cl12 C25 1.7632(15) . ?
C25 H25A 0.9900 . ?
C25 H25B 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
Cl1 Zr P 174.441(10) . . ?
Cl2 Zr Cl1 96.86(2) . . ?
Cl2 Zr P 87.197(19) . . ?
N1 Zr Cl1 96.61(4) . . ?
N1 Zr Cl2 121.41(4) . . ?
N1 Zr P 78.00(4) . . ?
N1 Zr N2 115.62(4) . . ?
N2 Zr Cl1 100.02(3) . . ?
N2 Zr Cl2 117.53(4) . . ?
N2 Zr P 81.35(3) . . ?
C1 P Zr 114.11(4) . . ?
C1 P C4 103.36(6) . . ?
C4 P Zr 103.98(4) . . ?
C7 P Zr 124.62(4) . . ?
C7 P C1 105.76(6) . . ?
C7 P C4 102.31(5) . . ?
C3 N1 Zr 110.88(7) . . ?
C13 N1 Zr 131.70(8) . . ?
C13 N1 C3 117.38(9) . . ?
C6 N2 Zr 119.42(7) . . ?
C19 N2 Zr 122.41(7) . . ?
C19 N2 C6 117.22(9) . . ?
P C1 H1A 109.1 . . ?
P C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 P 112.52(8) . . ?
C2 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C3 C2 C1 114.17(9) . . ?
C3 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
N1 C3 C2 113.85(9) . . ?
N1 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
C2 C3 H3A 108.8 . . ?
C2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
P C4 H4A 108.8 . . ?
P C4 H4B 108.8 . . ?
H4A C4 H4B 107.6 . . ?
C5 C4 P 114.01(8) . . ?
C5 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
C4 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
C4 C5 C6 113.44(9) . . ?
H5A C5 H5B 107.7 . . ?
C6 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
N2 C6 C5 114.64(10) . . ?
N2 C6 H6A 108.6 . . ?
N2 C6 H6B 108.6 . . ?
C5 C6 H6A 108.6 . . ?
C5 C6 H6B 108.6 . . ?
H6A C6 H6B 107.6 . . ?
C8 C7 P 119.15(9) . . ?
C8 C7 C12 119.19(11) . . ?
C12 C7 P 121.50(9) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 C7 120.48(11) . . ?
C9 C8 H8 119.8 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 120.02(11) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 120.1 . . ?
C9 C10 C11 119.85(11) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 119.8 . . ?
C12 C11 C10 120.40(11) . . ?
C12 C11 H11 119.8 . . ?
C7 C12 H12 120.0 . . ?
C11 C12 C7 120.04(11) . . ?
C11 C12 H12 120.0 . . ?
N1 C13 C14 123.29(10) . . ?
N1 C13 C18 118.92(10) . . ?
C14 C13 C18 117.78(10) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 C13 120.45(11) . . ?
C15 C14 H14 119.8 . . ?
C14 C15 H15 119.4 . . ?
C16 C15 C14 121.13(11) . . ?
C16 C15 H15 119.4 . . ?
C15 C16 H16 120.6 . . ?
C15 C16 C17 118.78(11) . . ?
C17 C16 H16 120.6 . . ?
C16 C17 H17 119.7 . . ?
C18 C17 C16 120.69(11) . . ?
C18 C17 H17 119.7 . . ?
C13 C18 H18 119.5 . . ?
C17 C18 C13 121.09(11) . . ?
C17 C18 H18 119.5 . . ?
N2 C19 C20 118.67(10) . . ?
C24 C19 N2 123.93(10) . . ?
C24 C19 C20 117.38(10) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 C19 121.43(11) . . ?
C21 C20 H20 119.3 . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C22 120.62(11) . . ?
C22 C21 H21 119.7 . . ?
C21 C22 H22 120.7 . . ?
C23 C22 C21 118.64(11) . . ?
C23 C22 H22 120.7 . . ?
C22 C23 H23 119.3 . . ?
C22 C23 C24 121.40(11) . . ?
C24 C23 H23 119.3 . . ?
C19 C24 H24 119.8 . . ?
C23 C24 C19 120.46(11) . . ?
C23 C24 H24 119.8 . . ?
Cl11 C25 H25A 109.2 . . ?
Cl11 C25 H25B 109.2 . . ?
Cl12 C25 Cl11 111.93(7) . . ?
Cl12 C25 H25A 109.2 . . ?
Cl12 C25 H25B 109.2 . . ?
H25A C25 H25B 107.9 . . ?

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
Zr P C1 C2 -33.71(9) . . . . ?
Zr P C4 C5 -55.25(9) . . . . ?
Zr P C7 C8 19.91(11) . . . . ?
Zr P C7 C12 -164.85(8) . . . . ?
Zr N1 C3 C2 103.80(9) . . . . ?
Zr N1 C13 C14 -177.78(8) . . . . ?
Zr N1 C13 C18 3.25(15) . . . . ?
Zr N2 C6 C5 85.30(11) . . . . ?
Zr N2 C19 C20 19.13(14) . . . . ?
Zr N2 C19 C24 -159.99(9) . . . . ?
P C1 C2 C3 45.98(12) . . . . ?
P C4 C5 C6 66.69(12) . . . . ?
P C7 C8 C9 174.05(9) . . . . ?
P C7 C12 C11 -174.70(9) . . . . ?
N1 C13 C14 C15 178.78(10) . . . . ?
N1 C13 C18 C17 -178.13(10) . . . . ?
N2 C19 C20 C21 -176.31(11) . . . . ?
N2 C19 C24 C23 177.39(11) . . . . ?
C1 P C4 C5 -174.71(8) . . . . ?
C1 P C7 C8 155.20(9) . . . . ?
C1 P C7 C12 -29.56(11) . . . . ?
C1 C2 C3 N1 -82.29(12) . . . . ?
C3 N1 C13 C14 4.66(15) . . . . ?
C3 N1 C13 C18 -174.31(10) . . . . ?
C4 P C1 C2 78.52(9) . . . . ?
C4 P C7 C8 -96.90(10) . . . . ?
C4 P C7 C12 78.34(10) . . . . ?
C4 C5 C6 N2 -75.40(12) . . . . ?
C6 N2 C19 C20 -172.11(10) . . . . ?
C6 N2 C19 C24 8.77(16) . . . . ?
C7 P C1 C2 -174.34(8) . . . . ?
C7 P C4 C5 75.56(9) . . . . ?
C7 C8 C9 C10 0.78(18) . . . . ?
C8 C7 C12 C11 0.54(17) . . . . ?
C8 C9 C10 C11 0.52(18) . . . . ?
C9 C10 C11 C12 -1.28(18) . . . . ?
C10 C11 C12 C7 0.75(18) . . . . ?
C12 C7 C8 C9 -1.30(18) . . . . ?
C13 N1 C3 C2 -78.16(12) . . . . ?
C13 C14 C15 C16 -0.11(18) . . . . ?
C14 C13 C18 C17 2.85(16) . . . . ?
C14 C15 C16 C17 1.92(18) . . . . ?
C15 C16 C17 C18 -1.32(17) . . . . ?
C16 C17 C18 C13 -1.09(17) . . . . ?
C18 C13 C14 C15 -2.24(16) . . . . ?
C19 N2 C6 C5 -83.81(12) . . . . ?
C19 C20 C21 C22 -1.71(18) . . . . ?
C20 C19 C24 C23 -1.74(16) . . . . ?
C20 C21 C22 C23 -0.63(18) . . . . ?
C21 C22 C23 C24 1.75(18) . . . . ?
C22 C23 C24 C19 -0.54(18) . . . . ?
C24 C19 C20 C21 2.86(17) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            CCD-PXL-KAF2
####################################################################### 
# 
# 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_ba_tk10
_database_code_depnum_ccdc_archive 'CCDC 1440952'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;
_audit_creation_date             
;
'Mon Jul 06 15:49:16 2015'
;

_audit_block_code                ba_tk10
_audit_block_refno               2476
_audit_block_usercomment         'NPNHfCl2 colourless block'


_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C24 H27 Cl2 Hf N2 P, C H2 Cl2'
_chemical_formula_sum            'C25 H29 Cl4 Hf N2 P'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         708.76
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      120(1)
_chemical_oxdiff_formula         'C25 h29 Cl4 Hf1 N2 P1'
_chemical_oxdiff_usercomment     'NPNHfCl2 colourless block'
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'
Hf Hf -0.5830 6.1852 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration .

_space_group_name_Hall           '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.58828(12)
_cell_length_b                   11.7688(2)
_cell_length_c                   14.5396(3)
_cell_angle_alpha                66.6471(16)
_cell_angle_beta                 84.8482(13)
_cell_angle_gamma                75.6062(13)
_cell_volume                     1306.77(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    25862
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      32.1220
_cell_measurement_theta_min      3.8900
_shelx_estimated_absorpt_T_max   0.663
_shelx_estimated_absorpt_T_min   0.663
_exptl_absorpt_coefficient_mu    4.479
_exptl_absorpt_correction_T_max  0.567
_exptl_absorpt_correction_T_min  0.436
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.143
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47274
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.435
_diffrn_reflns_theta_min         3.454
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -8.00   77.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224 -113.0000  152.0000 170

#__ type_ start__ end____ width___ exp.time_
  2 omega   -3.00   56.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   77.0000 -120.0000 118

#__ type_ start__ end____ width___ exp.time_
  3 omega  -38.00   38.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224  -57.0000  -30.0000 152

#__ type_ start__ end____ width___ exp.time_
  4 omega   47.00   74.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224  178.0000  -30.0000 54

#__ type_ start__ end____ width___ exp.time_
  5 omega   35.00  102.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224  178.0000  150.0000 134

#__ type_ start__ end____ width___ exp.time_
  6 omega    3.00   38.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   77.0000   60.0000 70

#__ type_ start__ end____ width___ exp.time_
  7 omega  -21.00   28.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224  -19.0000   90.0000 98

#__ type_ start__ end____ width___ exp.time_
  8 omega   -3.00   90.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   77.0000  -30.0000 186

#__ type_ start__ end____ width___ exp.time_
  9 omega   -2.00   53.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   77.0000  120.0000 110

#__ type_ start__ end____ width___ exp.time_
 10 omega    2.00   99.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   38.0000  -60.0000 194

#__ type_ start__ end____ width___ exp.time_
 11 omega  -43.00   53.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224  -77.0000 -150.0000 192

#__ type_ start__ end____ width___ exp.time_
 12 omega  -12.00   69.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224  -99.0000  -30.0000 162

#__ type_ start__ end____ width___ exp.time_
 13 omega    7.00   89.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   57.0000 -150.0000 164

#__ type_ start__ end____ width___ exp.time_
 14 omega  -13.00  100.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   19.0000  150.0000 226

#__ type_ start__ end____ width___ exp.time_
 15 omega    7.00   96.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   57.0000  -60.0000 178

#__ type_ start__ end____ width___ exp.time_
 16 omega   34.00  104.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224 -178.0000    0.0000 140

#__ type_ start__ end____ width___ exp.time_
 17 omega    7.00   96.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   57.0000   30.0000 178

#__ type_ start__ end____ width___ exp.time_
 18 omega  -45.00   35.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224  -38.0000    0.0000 160

#__ type_ start__ end____ width___ exp.time_
 19 omega    2.00   99.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   38.0000  150.0000 194

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0301420000
_diffrn_orient_matrix_UB_12      -0.0224946000
_diffrn_orient_matrix_UB_13      0.0494835000
_diffrn_orient_matrix_UB_21      -0.0786408000
_diffrn_orient_matrix_UB_22      0.0187474000
_diffrn_orient_matrix_UB_23      0.0167489000
_diffrn_orient_matrix_UB_31      -0.0133430000
_diffrn_orient_matrix_UB_32      -0.0608221000
_diffrn_orient_matrix_UB_33      0.0097307000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus X-Ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8388
_reflns_number_total             8967
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.929
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         8967
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0231
_refine_ls_restrained_S_all      1.099
_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)+(0.0326P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0620
_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:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
Hf Hf 0.42671(2) 0.80581(2) 0.32579(2) 0.01279(3) Uani 1 1 d . . . . .
Cl1 Cl 0.70912(7) 0.71039(5) 0.31360(5) 0.02107(11) Uani 1 1 d . . . . .
Cl2 Cl 0.46433(8) 0.91204(6) 0.42877(4) 0.02309(12) Uani 1 1 d . . . . .
P P 0.10414(7) 0.89184(5) 0.34192(4) 0.01363(10) Uani 1 1 d . . . . .
N1 N 0.3512(2) 0.63980(17) 0.38466(14) 0.0157(4) Uani 1 1 d . . . . .
N2 N 0.3739(2) 0.91373(17) 0.17678(14) 0.0154(3) Uani 1 1 d . . . . .
C1 C 0.0149(3) 0.7908(2) 0.45399(17) 0.0174(4) Uani 1 1 d . . . . .
H1A H 0.0239 0.8166 0.5100 0.021 Uiso 1 1 calc R . . . .
H1B H -0.1008 0.8040 0.4412 0.021 Uiso 1 1 calc R . . . .
C2 C 0.0962(3) 0.6487(2) 0.48491(17) 0.0174(4) Uani 1 1 d . . . . .
H2A H 0.0601 0.6012 0.5529 0.021 Uiso 1 1 calc R . . . .
H2B H 0.0603 0.6173 0.4385 0.021 Uiso 1 1 calc R . . . .
C3 C 0.2803(3) 0.6199(2) 0.48491(16) 0.0160(4) Uani 1 1 d . . . . .
H3A H 0.3154 0.6750 0.5117 0.019 Uiso 1 1 calc R . . . .
H3B H 0.3224 0.5304 0.5305 0.019 Uiso 1 1 calc R . . . .
C4 C 0.0152(3) 0.8749(2) 0.23943(17) 0.0166(4) Uani 1 1 d . . . . .
H4A H 0.0326 0.7831 0.2535 0.020 Uiso 1 1 calc R . . . .
H4B H -0.1023 0.9105 0.2379 0.020 Uiso 1 1 calc R . . . .
C5 C 0.0831(3) 0.9405(2) 0.13630(16) 0.0163(4) Uani 1 1 d . . . . .
H5A H 0.0701 1.0315 0.1234 0.020 Uiso 1 1 calc R . . . .
H5B H 0.0199 0.9357 0.0848 0.020 Uiso 1 1 calc R . . . .
C6 C 0.2609(3) 0.8822(2) 0.12561(17) 0.0168(4) Uani 1 1 d . . . . .
H6A H 0.2772 0.7884 0.1523 0.020 Uiso 1 1 calc R . . . .
H6B H 0.2871 0.9111 0.0534 0.020 Uiso 1 1 calc R . . . .
C7 C 0.0077(3) 1.0549(2) 0.32522(17) 0.0161(4) Uani 1 1 d . . . . .
C8 C 0.0885(3) 1.1512(2) 0.27273(19) 0.0203(4) Uani 1 1 d . . . . .
H8 H 0.1962 1.1303 0.2521 0.024 Uiso 1 1 calc R . . . .
C9 C 0.0099(3) 1.2783(2) 0.25086(19) 0.0224(5) Uani 1 1 d . . . . .
H9 H 0.0641 1.3439 0.2144 0.027 Uiso 1 1 calc R . . . .
C10 C -0.1456(3) 1.3091(2) 0.28184(19) 0.0222(5) Uani 1 1 d . . . . .
H10 H -0.1981 1.3958 0.2666 0.027 Uiso 1 1 calc R . . . .
C11 C -0.2261(3) 1.2144(2) 0.33501(19) 0.0225(5) Uani 1 1 d . . . . .
H11 H -0.3330 1.2363 0.3565 0.027 Uiso 1 1 calc R . . . .
C12 C -0.1501(3) 1.0870(2) 0.35705(18) 0.0196(4) Uani 1 1 d . . . . .
H12 H -0.2053 1.0222 0.3936 0.024 Uiso 1 1 calc R . . . .
C13 C 0.3601(3) 0.5437(2) 0.34831(16) 0.0153(4) Uani 1 1 d . . . . .
C14 C 0.2947(3) 0.4370(2) 0.39897(17) 0.0171(4) Uani 1 1 d . . . . .
H14 H 0.2435 0.4264 0.4616 0.021 Uiso 1 1 calc R . . . .
C15 C 0.3046(3) 0.3473(2) 0.35815(18) 0.0201(4) Uani 1 1 d . . . . .
H15 H 0.2600 0.2757 0.3934 0.024 Uiso 1 1 calc R . . . .
C16 C 0.3782(3) 0.3599(2) 0.26670(18) 0.0203(4) Uani 1 1 d . . . . .
H16 H 0.3813 0.2991 0.2385 0.024 Uiso 1 1 calc R . . . .
C17 C 0.4469(3) 0.4625(2) 0.21731(18) 0.0197(4) Uani 1 1 d . . . . .
H17 H 0.4996 0.4713 0.1554 0.024 Uiso 1 1 calc R . . . .
C18 C 0.4397(3) 0.5528(2) 0.25746(17) 0.0176(4) Uani 1 1 d . . . . .
H18 H 0.4892 0.6219 0.2231 0.021 Uiso 1 1 calc R . . . .
C19 C 0.4195(3) 1.0301(2) 0.12439(16) 0.0151(4) Uani 1 1 d . . . . .
C20 C 0.5423(3) 1.0562(2) 0.16538(17) 0.0197(4) Uani 1 1 d . . . . .
H20 H 0.5961 0.9935 0.2249 0.024 Uiso 1 1 calc R . . . .
C21 C 0.5864(3) 1.1717(2) 0.12065(18) 0.0211(5) Uani 1 1 d . . . . .
H21 H 0.6679 1.1880 0.1506 0.025 Uiso 1 1 calc R . . . .
C22 C 0.5121(3) 1.2637(2) 0.03234(19) 0.0227(5) Uani 1 1 d . . . . .
H22 H 0.5414 1.3431 0.0021 0.027 Uiso 1 1 calc R . . . .
C23 C 0.3948(3) 1.2382(2) -0.01103(18) 0.0212(5) Uani 1 1 d . . . . .
H23 H 0.3455 1.3000 -0.0723 0.025 Uiso 1 1 calc R . . . .
C24 C 0.3478(3) 1.1229(2) 0.03392(17) 0.0181(4) Uani 1 1 d . . . . .
H24 H 0.2669 1.1072 0.0032 0.022 Uiso 1 1 calc R . . . .
Cl11 Cl 0.20059(8) 0.52373(6) 0.00270(5) 0.02704(13) Uani 1 1 d . . . . .
Cl12 Cl 0.00473(9) 0.64032(7) 0.13192(5) 0.03112(14) Uani 1 1 d . . . . .
C25 C 0.0707(3) 0.6631(2) 0.0089(2) 0.0287(6) Uani 1 1 d . . . . .
H25A H 0.1277 0.7330 -0.0159 0.034 Uiso 1 1 calc R . . . .
H25B H -0.0237 0.6887 -0.0353 0.034 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
Hf Cl1 2.4293(6) . ?
Hf Cl2 2.3835(6) . ?
Hf P 2.7262(6) . ?
Hf N1 2.0432(18) . ?
Hf N2 2.0545(18) . ?
P C1 1.830(2) . ?
P C4 1.833(2) . ?
P C7 1.817(2) . ?
N1 C3 1.480(3) . ?
N1 C13 1.409(3) . ?
N2 C6 1.470(3) . ?
N2 C19 1.412(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.538(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.532(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.528(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.532(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.400(3) . ?
C7 C12 1.402(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.398(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.378(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.385(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.395(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.406(3) . ?
C13 C18 1.409(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.385(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.389(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.383(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.388(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.408(3) . ?
C19 C24 1.405(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.387(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.389(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.384(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.397(3) . ?
C24 H24 0.9500 . ?
Cl11 C25 1.770(3) . ?
Cl12 C25 1.762(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 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
Cl1 Hf P 174.694(18) . . ?
Cl2 Hf Cl1 96.50(2) . . ?
Cl2 Hf P 87.41(2) . . ?
N1 Hf Cl1 96.64(6) . . ?
N1 Hf Cl2 121.25(6) . . ?
N1 Hf P 78.23(5) . . ?
N1 Hf N2 115.79(8) . . ?
N2 Hf Cl1 99.68(5) . . ?
N2 Hf Cl2 117.82(6) . . ?
N2 Hf P 81.55(5) . . ?
C1 P Hf 114.25(8) . . ?
C1 P C4 103.39(11) . . ?
C4 P Hf 104.46(8) . . ?
C7 P Hf 124.05(8) . . ?
C7 P C1 105.95(10) . . ?
C7 P C4 102.11(10) . . ?
C3 N1 Hf 111.19(14) . . ?
C13 N1 Hf 131.67(15) . . ?
C13 N1 C3 117.10(18) . . ?
C6 N2 Hf 119.32(14) . . ?
C19 N2 Hf 122.91(15) . . ?
C19 N2 C6 116.92(18) . . ?
P C1 H1A 109.1 . . ?
P C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 P 112.49(15) . . ?
C2 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C3 C2 C1 114.01(18) . . ?
C3 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
N1 C3 C2 113.74(18) . . ?
N1 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
C2 C3 H3A 108.8 . . ?
C2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
P C4 H4A 108.7 . . ?
P C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C5 C4 P 114.16(15) . . ?
C5 C4 H4A 108.7 . . ?
C5 C4 H4B 108.7 . . ?
C4 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
C4 C5 C6 113.52(18) . . ?
H5A C5 H5B 107.7 . . ?
C6 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
N2 C6 C5 114.93(18) . . ?
N2 C6 H6A 108.5 . . ?
N2 C6 H6B 108.5 . . ?
C5 C6 H6A 108.5 . . ?
C5 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
C8 C7 P 119.06(17) . . ?
C8 C7 C12 119.5(2) . . ?
C12 C7 P 121.28(18) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 C7 119.7(2) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.4(2) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 119.8 . . ?
C9 C10 C11 120.4(2) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.1(2) . . ?
C12 C11 H11 120.0 . . ?
C7 C12 H12 120.0 . . ?
C11 C12 C7 119.9(2) . . ?
C11 C12 H12 120.0 . . ?
C14 C13 N1 123.2(2) . . ?
C14 C13 C18 117.6(2) . . ?
C18 C13 N1 119.2(2) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 C13 120.4(2) . . ?
C15 C14 H14 119.8 . . ?
C14 C15 H15 119.3 . . ?
C14 C15 C16 121.4(2) . . ?
C16 C15 H15 119.3 . . ?
C15 C16 H16 120.5 . . ?
C17 C16 C15 118.9(2) . . ?
C17 C16 H16 120.5 . . ?
C16 C17 H17 119.7 . . ?
C16 C17 C18 120.6(2) . . ?
C18 C17 H17 119.7 . . ?
C13 C18 H18 119.4 . . ?
C17 C18 C13 121.1(2) . . ?
C17 C18 H18 119.4 . . ?
C20 C19 N2 118.5(2) . . ?
C24 C19 N2 123.9(2) . . ?
C24 C19 C20 117.7(2) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 C19 121.3(2) . . ?
C21 C20 H20 119.3 . . ?
C20 C21 H21 119.8 . . ?
C20 C21 C22 120.4(2) . . ?
C22 C21 H21 119.8 . . ?
C21 C22 H22 120.4 . . ?
C23 C22 C21 119.2(2) . . ?
C23 C22 H22 120.4 . . ?
C22 C23 H23 119.5 . . ?
C22 C23 C24 121.0(2) . . ?
C24 C23 H23 119.5 . . ?
C19 C24 H24 119.8 . . ?
C23 C24 C19 120.4(2) . . ?
C23 C24 H24 119.8 . . ?
Cl11 C25 H25A 109.2 . . ?
Cl11 C25 H25B 109.2 . . ?
Cl12 C25 Cl11 111.96(15) . . ?
Cl12 C25 H25A 109.2 . . ?
Cl12 C25 H25B 109.2 . . ?
H25A C25 H25B 107.9 . . ?

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
Hf P C1 C2 -34.05(19) . . . . ?
Hf P C4 C5 -54.40(17) . . . . ?
Hf P C7 C8 20.2(2) . . . . ?
Hf P C7 C12 -164.73(15) . . . . ?
Hf N1 C3 C2 103.27(18) . . . . ?
Hf N1 C13 C14 -177.49(17) . . . . ?
Hf N1 C13 C18 3.3(3) . . . . ?
Hf N2 C6 C5 85.3(2) . . . . ?
Hf N2 C19 C20 18.5(3) . . . . ?
Hf N2 C19 C24 -160.56(17) . . . . ?
P C1 C2 C3 46.3(2) . . . . ?
P C4 C5 C6 65.4(2) . . . . ?
P C7 C8 C9 173.82(19) . . . . ?
P C7 C12 C11 -174.11(18) . . . . ?
N1 C13 C14 C15 178.7(2) . . . . ?
N1 C13 C18 C17 -178.0(2) . . . . ?
N2 C19 C20 C21 -176.3(2) . . . . ?
N2 C19 C24 C23 177.1(2) . . . . ?
C1 P C4 C5 -174.24(16) . . . . ?
C1 P C7 C8 155.34(19) . . . . ?
C1 P C7 C12 -29.6(2) . . . . ?
C1 C2 C3 N1 -82.0(2) . . . . ?
C3 N1 C13 C14 4.9(3) . . . . ?
C3 N1 C13 C18 -174.29(19) . . . . ?
C4 P C1 C2 78.83(18) . . . . ?
C4 P C7 C8 -96.7(2) . . . . ?
C4 P C7 C12 78.3(2) . . . . ?
C4 C5 C6 N2 -75.0(2) . . . . ?
C6 N2 C19 C20 -172.2(2) . . . . ?
C6 N2 C19 C24 8.8(3) . . . . ?
C7 P C1 C2 -174.17(16) . . . . ?
C7 P C4 C5 75.89(18) . . . . ?
C7 C8 C9 C10 0.9(4) . . . . ?
C8 C7 C12 C11 0.9(3) . . . . ?
C8 C9 C10 C11 0.0(4) . . . . ?
C9 C10 C11 C12 -0.4(4) . . . . ?
C10 C11 C12 C7 -0.1(4) . . . . ?
C12 C7 C8 C9 -1.3(4) . . . . ?
C13 N1 C3 C2 -78.6(2) . . . . ?
C13 C14 C15 C16 -0.1(4) . . . . ?
C14 C13 C18 C17 2.8(3) . . . . ?
C14 C15 C16 C17 1.9(4) . . . . ?
C15 C16 C17 C18 -1.3(4) . . . . ?
C16 C17 C18 C13 -1.1(3) . . . . ?
C18 C13 C14 C15 -2.2(3) . . . . ?
C19 N2 C6 C5 -84.4(2) . . . . ?
C19 C20 C21 C22 -1.5(4) . . . . ?
C20 C19 C24 C23 -2.0(3) . . . . ?
C20 C21 C22 C23 -0.7(4) . . . . ?
C21 C22 C23 C24 1.5(4) . . . . ?
C22 C23 C24 C19 -0.2(4) . . . . ?
C24 C19 C20 C21 2.8(3) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
7 -9 3 0.1022 7.0000 -9.0000 3.0000 0.5619 -0.6690 0.4832
-9 -14 -7 0.1061 -9.0000 -14.0000 -7.0000 -0.3027 0.3281 0.9035
9 14 7 0.1061 9.0000 14.0000 7.0000 0.3027 -0.3281 -0.9035
-9 6 -4 0.0898 -9.0000 6.0000 -4.0000 -0.6042 0.7533 -0.2838
1 6 20 0.0713 1.0000 6.0000 20.0000 0.8848 0.3688 -0.1837
-1 -6 -20 0.0713 -1.0000 -6.0000 -20.0000 -0.8848 -0.3688 0.1837
-4 -14 4 0.1287 -4.0000 -14.0000 4.0000 0.3923 0.1191 0.9438
4 14 -4 0.1287 4.0000 14.0000 -4.0000 -0.3923 -0.1191 -0.9438
-7 10 8 0.0957 -7.0000 10.0000 8.0000 -0.0401 0.8720 -0.4370
9 13 1 0.1052 9.0000 13.0000 1.0000 0.0283 -0.4473 -0.9010
10 -4 -6 0.1232 10.0000 -4.0000 -6.0000 0.0945 -0.9619 0.0515
-9 -7 9 0.1150 -9.0000 -7.0000 9.0000 0.3315 0.7273 0.6334
8 11 -4 0.1024 8.0000 11.0000 -4.0000 -0.2042 -0.4899 -0.8147
8 -1 -14 0.1196 8.0000 -1.0000 -14.0000 -0.4291 -0.8824 -0.1822
0 -16 -10 0.1304 0.0000 -16.0000 -10.0000 -0.1349 -0.4674 0.8758
7 -5 11 0.1038 7.0000 -5.0000 11.0000 0.8678 -0.4600 0.3177

_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            8.58828(12)
_cell_oxdiff_length_b            11.7688(2)
_cell_oxdiff_length_c            14.5396(2)
_cell_oxdiff_angle_alpha         66.6471(16)
_cell_oxdiff_angle_beta          84.8482(13)
_cell_oxdiff_angle_gamma         75.6062(13)
_cell_oxdiff_volume              1306.77(4)
_cell_oxdiff_measurement_reflns_used 25862
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ba_sb13
_database_code_depnum_ccdc_archive 'CCDC 1440953'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;
_audit_creation_date             2014-05-29

_audit_block_code                ba_sb13-
_audit_block_refno               2059-
_audit_block_usercomment         sb-mh30


_shelxl_version_number           2014-3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H47 N4 P Si2 Zr'
_chemical_formula_sum            'C30 H47 N4 P Si2 Zr'
_chemical_properties_physical    air-sensitive
_chemical_formula_weight         642.08
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      100(1)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.232(4)
_cell_length_b                   11.587(5)
_cell_length_c                   15.894(7)
_cell_angle_alpha                87.520(8)
_cell_angle_beta                 74.549(10)
_cell_angle_gamma                66.993(11)
_cell_volume                     1667.9(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8110
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.03
_cell_measurement_theta_min      2.25
_shelx_estimated_absorpt_T_max   0.920
_shelx_estimated_absorpt_T_min   0.887
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6979

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43380
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.544
_diffrn_reflns_theta_min         1.332
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9790
_reflns_number_total             11248
_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 8.x (Bruker AXS, 1997-2012). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT 8.x (Bruker AXS, 1997-2011)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-13); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         11248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0277
_refine_ls_restrained_S_all      1.042
_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)+(0.0260P)²+0.8428P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0666
_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:
 C1(H1A,H1B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16), C17(H17),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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 0.43051(2) 0.78818(2) 0.31214(2) 0.00843(3) Uani 1 1 d . . . . .
P P 0.51321(3) 0.72588(3) 0.12598(2) 0.01040(6) Uani 1 1 d . . . . .
Si1 Si 0.22239(4) 0.60444(3) 0.35857(2) 0.01203(7) Uani 1 1 d . . . . .
Si2 Si 0.33329(4) 1.10165(3) 0.26219(2) 0.01453(7) Uani 1 1 d . . . . .
N1 N 0.38372(11) 0.62611(9) 0.30650(6) 0.01043(18) Uani 1 1 d . . . . .
N2 N 0.31491(11) 0.95895(9) 0.25990(6) 0.01117(18) Uani 1 1 d . . . . .
N3 N 0.33512(12) 0.84910(10) 0.44204(7) 0.01306(19) Uani 1 1 d . . . . .
N4 N 0.64672(12) 0.73808(11) 0.31244(7) 0.0150(2) Uani 1 1 d . . . . .
C1 C 0.45599(14) 0.59643(11) 0.11589(8) 0.0130(2) Uani 1 1 d . . . . .
H1A H 0.3475 0.6255 0.1383 0.016 Uiso 1 1 calc R . . . .
H1B H 0.4853 0.5659 0.0538 0.016 Uiso 1 1 calc R . . . .
C2 C 0.38760(14) 0.85703(12) 0.07963(8) 0.0138(2) Uani 1 1 d . . . . .
H2A H 0.4218 0.9268 0.0718 0.017 Uiso 1 1 calc R . . . .
H2B H 0.3880 0.8290 0.0216 0.017 Uiso 1 1 calc R . . . .
C3 C 0.53055(13) 0.49259(11) 0.16854(8) 0.0124(2) Uani 1 1 d . . . . .
C4 C 0.49917(13) 0.51393(11) 0.26009(8) 0.0114(2) Uani 1 1 d . . . . .
C5 C 0.58444(14) 0.42096(12) 0.30504(8) 0.0152(2) Uani 1 1 d . . . . .
H5 H 0.5683 0.4355 0.3660 0.018 Uiso 1 1 calc R . . . .
C6 C 0.69199(15) 0.30802(12) 0.26275(9) 0.0190(3) Uani 1 1 d . . . . .
H6 H 0.7483 0.2466 0.2948 0.023 Uiso 1 1 calc R . . . .
C7 C 0.71725(15) 0.28495(12) 0.17355(9) 0.0190(3) Uani 1 1 d . . . . .
H7 H 0.7877 0.2066 0.1447 0.023 Uiso 1 1 calc R . . . .
C8 C 0.63816(15) 0.37787(12) 0.12713(9) 0.0165(2) Uani 1 1 d . . . . .
H8 H 0.6575 0.3632 0.0658 0.020 Uiso 1 1 calc R . . . .
C9 C 0.07887(15) 0.74852(13) 0.42489(9) 0.0192(3) Uani 1 1 d . . . . .
H9A H 0.1124 0.7654 0.4735 0.029 Uiso 1 1 calc GR . . . .
H9B H -0.0131 0.7360 0.4480 0.029 Uiso 1 1 calc GR . . . .
H9C H 0.0618 0.8200 0.3880 0.029 Uiso 1 1 calc GR . . . .
C10 C 0.14751(15) 0.56633(14) 0.27322(10) 0.0212(3) Uani 1 1 d . . . . .
H10A H 0.1141 0.6399 0.2395 0.032 Uiso 1 1 calc GR . . . .
H10B H 0.0643 0.5434 0.3015 0.032 Uiso 1 1 calc GR . . . .
H10C H 0.2249 0.4958 0.2339 0.032 Uiso 1 1 calc GR . . . .
C11 C 0.25306(16) 0.47426(13) 0.43465(10) 0.0227(3) Uani 1 1 d . . . . .
H11A H 0.3237 0.3951 0.4016 0.034 Uiso 1 1 calc GR . . . .
H11B H 0.1593 0.4666 0.4622 0.034 Uiso 1 1 calc GR . . . .
H11C H 0.2922 0.4930 0.4799 0.034 Uiso 1 1 calc GR . . . .
C12 C 0.23353(14) 0.90231(11) 0.13959(8) 0.0133(2) Uani 1 1 d . . . . .
C13 C 0.20198(13) 0.95287(11) 0.22548(8) 0.0116(2) Uani 1 1 d . . . . .
C14 C 0.05565(14) 0.99427(12) 0.27780(9) 0.0153(2) Uani 1 1 d . . . . .
H14 H 0.0318 1.0307 0.3351 0.018 Uiso 1 1 calc R . . . .
C15 C -0.05511(15) 0.98339(13) 0.24793(10) 0.0199(3) Uani 1 1 d . . . . .
H15 H -0.1531 1.0118 0.2848 0.024 Uiso 1 1 calc R . . . .
C16 C -0.02299(16) 0.93127(14) 0.16451(11) 0.0232(3) Uani 1 1 d . . . . .
H16 H -0.0981 0.9226 0.1441 0.028 Uiso 1 1 calc R . . . .
C17 C 0.12062(15) 0.89163(13) 0.11092(9) 0.0192(3) Uani 1 1 d . . . . .
H17 H 0.1425 0.8564 0.0535 0.023 Uiso 1 1 calc R . . . .
C18 C 0.15171(18) 1.23336(13) 0.31027(10) 0.0253(3) Uani 1 1 d . . . . .
H18A H 0.0851 1.2419 0.2739 0.038 Uiso 1 1 calc GR . . . .
H18B H 0.1663 1.3118 0.3125 0.038 Uiso 1 1 calc GR . . . .
H18C H 0.1085 1.2154 0.3696 0.038 Uiso 1 1 calc GR . . . .
C19 C 0.41178(18) 1.14308(14) 0.15040(10) 0.0244(3) Uani 1 1 d . . . . .
H19A H 0.5103 1.0785 0.1248 0.037 Uiso 1 1 calc GR . . . .
H19B H 0.4186 1.2246 0.1546 0.037 Uiso 1 1 calc GR . . . .
H19C H 0.3475 1.1479 0.1132 0.037 Uiso 1 1 calc GR . . . .
C20 C 0.46539(18) 1.08732(14) 0.32716(10) 0.0235(3) Uani 1 1 d . . . . .
H20A H 0.4242 1.0727 0.3878 0.035 Uiso 1 1 calc GR . . . .
H20B H 0.4823 1.1651 0.3259 0.035 Uiso 1 1 calc GR . . . .
H20C H 0.5591 1.0166 0.3019 0.035 Uiso 1 1 calc GR . . . .
C21 C 0.69020(14) 0.68947(13) 0.04511(8) 0.0148(2) Uani 1 1 d . . . . .
C22 C 0.75468(15) 0.59179(13) -0.01968(9) 0.0186(3) Uani 1 1 d . . . . .
H22 H 0.7069 0.5370 -0.0228 0.022 Uiso 1 1 calc R . . . .
C23 C 0.88911(16) 0.57349(16) -0.08026(9) 0.0251(3) Uani 1 1 d . . . . .
H23 H 0.9333 0.5053 -0.1235 0.030 Uiso 1 1 calc R . . . .
C24 C 0.95774(17) 0.65377(18) -0.07761(10) 0.0301(3) Uani 1 1 d . . . . .
H24 H 1.0484 0.6419 -0.1196 0.036 Uiso 1 1 calc R . . . .
C25 C 0.89473(19) 0.7522(2) -0.01364(11) 0.0355(4) Uani 1 1 d . . . . .
H25 H 0.9418 0.8080 -0.0120 0.043 Uiso 1 1 calc R . . . .
C26 C 0.76229(17) 0.76893(16) 0.04813(10) 0.0268(3) Uani 1 1 d . . . . .
H26 H 0.7206 0.8351 0.0927 0.032 Uiso 1 1 calc R . . . .
C27 C 0.22229(16) 0.96519(13) 0.48828(9) 0.0189(3) Uani 1 1 d . . . . .
H27A H 0.1900 1.0265 0.4459 0.028 Uiso 1 1 calc GR . . . .
H27B H 0.2626 0.9988 0.5261 0.028 Uiso 1 1 calc GR . . . .
H27C H 0.1380 0.9488 0.5241 0.028 Uiso 1 1 calc GR . . . .
C28 C 0.38460(16) 0.75614(14) 0.50368(9) 0.0204(3) Uani 1 1 d . . . . .
H28A H 0.3011 0.7381 0.5388 0.031 Uiso 1 1 calc GR . . . .
H28B H 0.4243 0.7891 0.5422 0.031 Uiso 1 1 calc GR . . . .
H28C H 0.4616 0.6787 0.4714 0.031 Uiso 1 1 calc GR . . . .
C29 C 0.77001(15) 0.63544(14) 0.25563(10) 0.0215(3) Uani 1 1 d . . . . .
H29A H 0.8158 0.5688 0.2914 0.032 Uiso 1 1 calc GR . . . .
H29B H 0.8431 0.6669 0.2221 0.032 Uiso 1 1 calc GR . . . .
H29C H 0.7339 0.6018 0.2153 0.032 Uiso 1 1 calc GR . . . .
C30 C 0.69926(16) 0.78322(14) 0.37593(9) 0.0209(3) Uani 1 1 d . . . . .
H30A H 0.6158 0.8492 0.4159 0.031 Uiso 1 1 calc GR . . . .
H30B H 0.7714 0.8174 0.3451 0.031 Uiso 1 1 calc GR . . . .
H30C H 0.7459 0.7134 0.4093 0.031 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
Zr P 2.8922(13) . ?
Zr N1 2.1223(13) . ?
Zr N2 2.1343(12) . ?
Zr N3 2.0561(13) . ?
Zr N4 2.0574(14) . ?
P C1 1.8373(14) . ?
P C2 1.8398(13) . ?
P C21 1.8219(14) . ?
Si1 N1 1.7467(12) . ?
Si1 C9 1.8617(15) . ?
Si1 C10 1.8689(15) . ?
Si1 C11 1.8735(15) . ?
Si2 N2 1.7385(13) . ?
Si2 C18 1.8690(16) . ?
Si2 C19 1.8707(16) . ?
Si2 C20 1.8640(16) . ?
N1 C4 1.4309(16) . ?
N2 C13 1.4294(16) . ?
N3 C27 1.4499(17) . ?
N3 C28 1.4571(17) . ?
N4 C29 1.4610(18) . ?
N4 C30 1.4614(17) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C3 1.5051(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C12 1.5050(18) . ?
C3 C4 1.4149(18) . ?
C3 C8 1.3993(18) . ?
C4 C5 1.4011(17) . ?
C5 H5 0.9500 . ?
C5 C6 1.3899(18) . ?
C6 H6 0.9500 . ?
C6 C7 1.390(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.3881(19) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.4134(18) . ?
C12 C17 1.3981(19) . ?
C13 C14 1.4047(18) . ?
C14 H14 0.9500 . ?
C14 C15 1.389(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.383(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.391(2) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.3899(19) . ?
C21 C26 1.396(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.396(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.375(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.388(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.393(2) . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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 Zr P 77.49(3) . . ?
N1 Zr N2 121.75(5) . . ?
N2 Zr P 75.62(4) . . ?
N3 Zr P 169.95(3) . . ?
N3 Zr N1 101.49(4) . . ?
N3 Zr N2 96.90(5) . . ?
N3 Zr N4 97.66(5) . . ?
N4 Zr P 92.00(3) . . ?
N4 Zr N1 110.60(5) . . ?
N4 Zr N2 120.97(4) . . ?
C1 P Zr 104.75(4) . . ?
C1 P C2 103.62(6) . . ?
C2 P Zr 106.78(5) . . ?
C21 P Zr 129.70(5) . . ?
C21 P C1 106.97(6) . . ?
C21 P C2 102.42(6) . . ?
N1 Si1 C9 111.76(6) . . ?
N1 Si1 C10 108.57(6) . . ?
N1 Si1 C11 112.91(6) . . ?
C9 Si1 C10 108.27(7) . . ?
C9 Si1 C11 106.67(7) . . ?
C10 Si1 C11 108.52(7) . . ?
N2 Si2 C18 111.50(7) . . ?
N2 Si2 C19 112.16(6) . . ?
N2 Si2 C20 108.29(6) . . ?
C18 Si2 C19 107.40(7) . . ?
C20 Si2 C18 110.53(8) . . ?
C20 Si2 C19 106.87(8) . . ?
Si1 N1 Zr 128.62(6) . . ?
C4 N1 Zr 118.48(8) . . ?
C4 N1 Si1 112.72(8) . . ?
Si2 N2 Zr 128.12(6) . . ?
C13 N2 Zr 113.25(8) . . ?
C13 N2 Si2 118.44(8) . . ?
C27 N3 Zr 134.21(9) . . ?
C27 N3 C28 110.52(11) . . ?
C28 N3 Zr 115.21(9) . . ?
C29 N4 Zr 123.40(9) . . ?
C29 N4 C30 109.40(11) . . ?
C30 N4 Zr 126.57(9) . . ?
P C1 H1A 110.2 . . ?
P C1 H1B 110.2 . . ?
H1A C1 H1B 108.5 . . ?
C3 C1 P 107.75(9) . . ?
C3 C1 H1A 110.2 . . ?
C3 C1 H1B 110.2 . . ?
P C2 H2A 109.6 . . ?
P C2 H2B 109.6 . . ?
H2A C2 H2B 108.2 . . ?
C12 C2 P 110.08(9) . . ?
C12 C2 H2A 109.6 . . ?
C12 C2 H2B 109.6 . . ?
C4 C3 C1 119.77(11) . . ?
C8 C3 C1 120.61(11) . . ?
C8 C3 C4 119.48(11) . . ?
C3 C4 N1 121.75(11) . . ?
C5 C4 N1 120.28(11) . . ?
C5 C4 C3 117.96(11) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 C4 121.73(12) . . ?
C6 C5 H5 119.1 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 120.01(12) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.15(12) . . ?
C8 C7 H7 120.4 . . ?
C3 C8 H8 119.2 . . ?
C7 C8 C3 121.53(12) . . ?
C7 C8 H8 119.2 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C2 120.82(11) . . ?
C17 C12 C2 119.75(12) . . ?
C17 C12 C13 119.41(12) . . ?
C12 C13 N2 121.71(11) . . ?
C14 C13 N2 120.35(11) . . ?
C14 C13 C12 117.92(12) . . ?
C13 C14 H14 119.1 . . ?
C15 C14 C13 121.76(13) . . ?
C15 C14 H14 119.1 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 120.08(13) . . ?
C16 C15 H15 120.0 . . ?
C15 C16 H16 120.4 . . ?
C15 C16 C17 119.21(13) . . ?
C17 C16 H16 120.4 . . ?
C12 C17 H17 119.2 . . ?
C16 C17 C12 121.60(13) . . ?
C16 C17 H17 119.2 . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si2 C20 H20A 109.5 . . ?
Si2 C20 H20B 109.5 . . ?
Si2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 P 124.79(11) . . ?
C22 C21 C26 118.68(12) . . ?
C26 C21 P 116.50(10) . . ?
C21 C22 H22 119.7 . . ?
C21 C22 C23 120.55(14) . . ?
C23 C22 H22 119.7 . . ?
C22 C23 H23 119.9 . . ?
C24 C23 C22 120.23(14) . . ?
C24 C23 H23 119.9 . . ?
C23 C24 H24 120.0 . . ?
C23 C24 C25 120.05(14) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 120.1 . . ?
C24 C25 C26 119.84(16) . . ?
C26 C25 H25 120.1 . . ?
C21 C26 H26 119.7 . . ?
C25 C26 C21 120.63(14) . . ?
C25 C26 H26 119.7 . . ?
N3 C27 H27A 109.5 . . ?
N3 C27 H27B 109.5 . . ?
N3 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N3 C28 H28A 109.5 . . ?
N3 C28 H28B 109.5 . . ?
N3 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N4 C29 H29A 109.5 . . ?
N4 C29 H29B 109.5 . . ?
N4 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N4 C30 H30A 109.5 . . ?
N4 C30 H30B 109.5 . . ?
N4 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 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
Zr P C1 C3 -56.76(9) . . . . ?
Zr P C2 C12 -40.31(9) . . . . ?
Zr P C21 C22 135.81(10) . . . . ?
Zr P C21 C26 -46.13(13) . . . . ?
Zr N1 C4 C3 -84.77(13) . . . . ?
Zr N1 C4 C5 95.64(12) . . . . ?
Zr N2 C13 C12 -83.91(12) . . . . ?
Zr N2 C13 C14 94.23(11) . . . . ?
P C1 C3 C4 62.65(13) . . . . ?
P C1 C3 C8 -112.95(12) . . . . ?
P C2 C12 C13 62.24(14) . . . . ?
P C2 C12 C17 -116.23(12) . . . . ?
P C21 C22 C23 178.24(11) . . . . ?
P C21 C26 C25 -176.92(14) . . . . ?
Si1 N1 C4 C3 99.62(12) . . . . ?
Si1 N1 C4 C5 -79.97(13) . . . . ?
Si2 N2 C13 C12 100.69(12) . . . . ?
Si2 N2 C13 C14 -81.17(13) . . . . ?
N1 C4 C5 C6 176.45(12) . . . . ?
N2 C13 C14 C15 -176.47(11) . . . . ?
C1 P C2 C12 69.98(10) . . . . ?
C1 P C21 C22 8.98(13) . . . . ?
C1 P C21 C26 -172.96(11) . . . . ?
C1 C3 C4 N1 8.49(17) . . . . ?
C1 C3 C4 C5 -171.90(11) . . . . ?
C1 C3 C8 C7 174.37(12) . . . . ?
C2 P C1 C3 -168.53(8) . . . . ?
C2 P C21 C22 -99.64(13) . . . . ?
C2 P C21 C26 78.42(13) . . . . ?
C2 C12 C13 N2 -2.29(17) . . . . ?
C2 C12 C13 C14 179.52(11) . . . . ?
C2 C12 C17 C16 179.42(12) . . . . ?
C3 C4 C5 C6 -3.17(19) . . . . ?
C4 C3 C8 C7 -1.24(19) . . . . ?
C4 C5 C6 C7 0.0(2) . . . . ?
C5 C6 C7 C8 2.6(2) . . . . ?
C6 C7 C8 C3 -2.0(2) . . . . ?
C8 C3 C4 N1 -175.87(11) . . . . ?
C8 C3 C4 C5 3.74(18) . . . . ?
C9 Si1 N1 Zr 0.84(9) . . . . ?
C9 Si1 N1 C4 175.90(9) . . . . ?
C10 Si1 N1 Zr 120.20(8) . . . . ?
C10 Si1 N1 C4 -64.75(10) . . . . ?
C11 Si1 N1 Zr -119.42(8) . . . . ?
C11 Si1 N1 C4 55.64(11) . . . . ?
C12 C13 C14 C15 1.74(18) . . . . ?
C13 C12 C17 C16 0.9(2) . . . . ?
C13 C14 C15 C16 -0.3(2) . . . . ?
C14 C15 C16 C17 -0.8(2) . . . . ?
C15 C16 C17 C12 0.5(2) . . . . ?
C17 C12 C13 N2 176.18(11) . . . . ?
C17 C12 C13 C14 -2.00(17) . . . . ?
C18 Si2 N2 Zr -126.07(8) . . . . ?
C18 Si2 N2 C13 48.56(11) . . . . ?
C19 Si2 N2 Zr 113.44(8) . . . . ?
C19 Si2 N2 C13 -71.93(11) . . . . ?
C20 Si2 N2 Zr -4.25(9) . . . . ?
C20 Si2 N2 C13 170.38(9) . . . . ?
C21 P C1 C3 83.69(10) . . . . ?
C21 P C2 C12 -178.86(9) . . . . ?
C21 C22 C23 C24 -1.4(2) . . . . ?
C22 C21 C26 C25 1.3(2) . . . . ?
C22 C23 C24 C25 1.1(3) . . . . ?
C23 C24 C25 C26 0.4(3) . . . . ?
C24 C25 C26 C21 -1.6(3) . . . . ?
C26 C21 C22 C23 0.2(2) . . . . ?

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2

_chemical_absolute_configuration .

_diffrn_ambient_environment      'perfluoro polyether oil'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            CCD-PXL-KAF2
####################################################################### 
# 
# 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_ba_sb12
_database_code_depnum_ccdc_archive 'CCDC 1440954'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;
_audit_creation_date             2015-12-03

_audit_block_code                ba_sb12
_audit_block_refno               2057
_audit_block_usercomment         sb-mh25


_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H47 Hf N4 P Si2'
_chemical_formula_sum            'C30 H47 Hf N4 P Si2'
_chemical_properties_physical    moisture-sensitive
_chemical_formula_weight         729.35
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      100(1)
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'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2

_chemical_absolute_configuration .

_space_group_name_Hall           '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.220(5)
_cell_length_b                   11.565(7)
_cell_length_c                   15.890(9)
_cell_angle_alpha                87.543(9)
_cell_angle_beta                 74.477(8)
_cell_angle_gamma                67.140(11)
_cell_volume                     1663.6(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7985
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.31
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   0.590
_shelx_estimated_absorpt_T_min   0.483
_exptl_absorpt_coefficient_mu    3.280
_exptl_absorpt_correction_T_max  0.5259
_exptl_absorpt_correction_T_min  0.4199

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41466
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.478
_diffrn_reflns_theta_min         2.248
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10393
_reflns_number_total             11185
_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 (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        
'SAINT V8.34A (Bruker AXS, 1997-2013),SADABS-2012_1 (Sheldrick and Bruker AXS, 1997-2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         1.805
_refine_diff_density_min         -1.596
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         11185
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0195
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0199P)²+1.2820P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0472
_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:
 C1(H1A,H1B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16), C17(H17),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
Hf Hf 0.43017(2) 0.78841(2) 0.31123(2) 0.00833(2) Uani 1 1 d . . . . .
P P 0.51253(5) 0.72665(4) 0.12620(3) 0.01033(7) Uani 1 1 d . . . . .
Si1 Si 0.22113(5) 0.60579(4) 0.35891(3) 0.01187(8) Uani 1 1 d . . . . .
Si2 Si 0.33275(6) 1.10168(5) 0.26295(3) 0.01412(9) Uani 1 1 d . . . . .
N1 N 0.38276(15) 0.62802(13) 0.30652(9) 0.0103(2) Uani 1 1 d . . . . .
N2 N 0.31454(15) 0.95845(13) 0.26045(9) 0.0108(2) Uani 1 1 d . . . . .
N3 N 0.33690(16) 0.84676(14) 0.44090(9) 0.0133(3) Uani 1 1 d . . . . .
N4 N 0.64529(16) 0.73856(15) 0.31077(10) 0.0147(3) Uani 1 1 d . . . . .
C1 C 0.45523(19) 0.59719(16) 0.11583(11) 0.0128(3) Uani 1 1 d . . . . .
H1A H 0.3467 0.6262 0.1382 0.015 Uiso 1 1 calc R . . . .
H1B H 0.4848 0.5667 0.0536 0.015 Uiso 1 1 calc R . . . .
C2 C 0.38734(19) 0.85787(16) 0.07974(11) 0.0139(3) Uani 1 1 d . . . . .
H2A H 0.4217 0.9277 0.0720 0.017 Uiso 1 1 calc R . . . .
H2B H 0.3880 0.8299 0.0216 0.017 Uiso 1 1 calc R . . . .
C3 C 0.52966(18) 0.49320(15) 0.16857(11) 0.0123(3) Uani 1 1 d . . . . .
C4 C 0.49791(18) 0.51535(15) 0.26004(11) 0.0115(3) Uani 1 1 d . . . . .
C5 C 0.58310(19) 0.42259(16) 0.30534(12) 0.0146(3) Uani 1 1 d . . . . .
H5 H 0.5670 0.4376 0.3663 0.018 Uiso 1 1 calc R . . . .
C6 C 0.6904(2) 0.30935(17) 0.26330(12) 0.0184(3) Uani 1 1 d . . . . .
H6 H 0.7467 0.2482 0.2955 0.022 Uiso 1 1 calc R . . . .
C7 C 0.7154(2) 0.28556(17) 0.17423(13) 0.0192(3) Uani 1 1 d . . . . .
H7 H 0.7856 0.2070 0.1456 0.023 Uiso 1 1 calc R . . . .
C8 C 0.6363(2) 0.37824(16) 0.12764(12) 0.0163(3) Uani 1 1 d . . . . .
H8 H 0.6553 0.3630 0.0664 0.020 Uiso 1 1 calc R . . . .
C9 C 0.0766(2) 0.74946(17) 0.42508(13) 0.0188(3) Uani 1 1 d . . . . .
H9A H 0.1104 0.7680 0.4731 0.028 Uiso 1 1 calc GR . . . .
H9B H -0.0145 0.7355 0.4491 0.028 Uiso 1 1 calc GR . . . .
H9C H 0.0578 0.8206 0.3878 0.028 Uiso 1 1 calc GR . . . .
C10 C 0.1470(2) 0.56664(19) 0.27352(13) 0.0208(4) Uani 1 1 d . . . . .
H10A H 0.1124 0.6403 0.2401 0.031 Uiso 1 1 calc GR . . . .
H10B H 0.0646 0.5424 0.3017 0.031 Uiso 1 1 calc GR . . . .
H10C H 0.2251 0.4967 0.2339 0.031 Uiso 1 1 calc GR . . . .
C11 C 0.2519(2) 0.47576(18) 0.43510(14) 0.0220(4) Uani 1 1 d . . . . .
H11A H 0.3222 0.3965 0.4020 0.033 Uiso 1 1 calc GR . . . .
H11B H 0.1580 0.4682 0.4631 0.033 Uiso 1 1 calc GR . . . .
H11C H 0.2917 0.4946 0.4801 0.033 Uiso 1 1 calc GR . . . .
C12 C 0.23303(18) 0.90309(16) 0.13954(11) 0.0130(3) Uani 1 1 d . . . . .
C13 C 0.20145(18) 0.95292(15) 0.22560(11) 0.0115(3) Uani 1 1 d . . . . .
C14 C 0.05491(19) 0.99459(16) 0.27792(12) 0.0154(3) Uani 1 1 d . . . . .
H14 H 0.0312 1.0307 0.3354 0.018 Uiso 1 1 calc R . . . .
C15 C -0.0562(2) 0.98448(17) 0.24794(13) 0.0193(4) Uani 1 1 d . . . . .
H15 H -0.1543 1.0130 0.2849 0.023 Uiso 1 1 calc R . . . .
C16 C -0.0239(2) 0.93272(19) 0.16397(15) 0.0231(4) Uani 1 1 d . . . . .
H16 H -0.0991 0.9245 0.1433 0.028 Uiso 1 1 calc R . . . .
C17 C 0.1198(2) 0.89301(18) 0.11052(13) 0.0193(3) Uani 1 1 d . . . . .
H17 H 0.1417 0.8582 0.0529 0.023 Uiso 1 1 calc R . . . .
C18 C 0.1514(2) 1.23340(18) 0.31116(15) 0.0250(4) Uani 1 1 d . . . . .
H18A H 0.0845 1.2416 0.2751 0.038 Uiso 1 1 calc GR . . . .
H18B H 0.1662 1.3120 0.3130 0.038 Uiso 1 1 calc GR . . . .
H18C H 0.1085 1.2157 0.3707 0.038 Uiso 1 1 calc GR . . . .
C19 C 0.4110(2) 1.1437(2) 0.15102(13) 0.0237(4) Uani 1 1 d . . . . .
H19A H 0.5093 1.0790 0.1251 0.036 Uiso 1 1 calc GR . . . .
H19B H 0.4185 1.2251 0.1553 0.036 Uiso 1 1 calc GR . . . .
H19C H 0.3462 1.1492 0.1141 0.036 Uiso 1 1 calc GR . . . .
C20 C 0.4652(2) 1.0876(2) 0.32775(14) 0.0233(4) Uani 1 1 d . . . . .
H20A H 0.4240 1.0731 0.3885 0.035 Uiso 1 1 calc GR . . . .
H20B H 0.4824 1.1654 0.3263 0.035 Uiso 1 1 calc GR . . . .
H20C H 0.5588 1.0168 0.3025 0.035 Uiso 1 1 calc GR . . . .
C21 C 0.68966(19) 0.69049(18) 0.04553(11) 0.0150(3) Uani 1 1 d . . . . .
C22 C 0.7552(2) 0.59192(18) -0.01918(12) 0.0191(3) Uani 1 1 d . . . . .
H22 H 0.7078 0.5364 -0.0218 0.023 Uiso 1 1 calc R . . . .
C23 C 0.8891(2) 0.5739(2) -0.07994(13) 0.0243(4) Uani 1 1 d . . . . .
H23 H 0.9332 0.5055 -0.1230 0.029 Uiso 1 1 calc R . . . .
C24 C 0.9579(2) 0.6546(2) -0.07791(14) 0.0294(5) Uani 1 1 d . . . . .
H24 H 1.0489 0.6423 -0.1198 0.035 Uiso 1 1 calc R . . . .
C25 C 0.8937(3) 0.7545(3) -0.01432(15) 0.0343(5) Uani 1 1 d . . . . .
H25 H 0.9401 0.8113 -0.0133 0.041 Uiso 1 1 calc R . . . .
C26 C 0.7613(2) 0.7710(2) 0.04782(14) 0.0259(4) Uani 1 1 d . . . . .
H26 H 0.7193 0.8377 0.0922 0.031 Uiso 1 1 calc R . . . .
C27 C 0.2239(2) 0.96292(17) 0.48692(12) 0.0183(3) Uani 1 1 d . . . . .
H27A H 0.1945 1.0250 0.4445 0.027 Uiso 1 1 calc GR . . . .
H27B H 0.2629 0.9953 0.5264 0.027 Uiso 1 1 calc GR . . . .
H27C H 0.1381 0.9470 0.5210 0.027 Uiso 1 1 calc GR . . . .
C28 C 0.3855(2) 0.75439(19) 0.50310(12) 0.0198(4) Uani 1 1 d . . . . .
H28A H 0.3021 0.7355 0.5376 0.030 Uiso 1 1 calc GR . . . .
H28B H 0.4234 0.7884 0.5423 0.030 Uiso 1 1 calc GR . . . .
H28C H 0.4638 0.6772 0.4712 0.030 Uiso 1 1 calc GR . . . .
C29 C 0.7697(2) 0.63682(19) 0.25376(13) 0.0206(4) Uani 1 1 d . . . . .
H29A H 0.8159 0.5702 0.2894 0.031 Uiso 1 1 calc GR . . . .
H29B H 0.8421 0.6694 0.2205 0.031 Uiso 1 1 calc GR . . . .
H29C H 0.7344 0.6025 0.2132 0.031 Uiso 1 1 calc GR . . . .
C30 C 0.6976(2) 0.78328(19) 0.37487(13) 0.0203(4) Uani 1 1 d . . . . .
H30A H 0.6142 0.8499 0.4145 0.030 Uiso 1 1 calc GR . . . .
H30B H 0.7710 0.8165 0.3443 0.030 Uiso 1 1 calc GR . . . .
H30C H 0.7425 0.7134 0.4087 0.030 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
Hf P 2.8724(16) . ?
Hf N1 2.1002(17) . ?
Hf N2 2.1175(16) . ?
Hf N3 2.0440(18) . ?
Hf N4 2.0428(18) . ?
P C1 1.8346(19) . ?
P C2 1.8402(18) . ?
P C21 1.8196(19) . ?
Si1 N1 1.7503(16) . ?
Si1 C9 1.860(2) . ?
Si1 C10 1.868(2) . ?
Si1 C11 1.872(2) . ?
Si2 N2 1.7404(17) . ?
Si2 C18 1.868(2) . ?
Si2 C19 1.873(2) . ?
Si2 C20 1.865(2) . ?
N1 C4 1.433(2) . ?
N2 C13 1.432(2) . ?
N3 C27 1.449(2) . ?
N3 C28 1.458(2) . ?
N4 C29 1.461(2) . ?
N4 C30 1.464(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C3 1.507(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C12 1.504(2) . ?
C3 C4 1.414(2) . ?
C3 C8 1.396(2) . ?
C4 C5 1.404(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.390(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.389(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.389(3) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.412(2) . ?
C12 C17 1.400(2) . ?
C13 C14 1.405(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.389(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.388(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.389(3) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.394(3) . ?
C21 C26 1.397(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.392(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.376(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.394(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.394(3) . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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 Hf P 77.89(4) . . ?
N1 Hf N2 121.86(6) . . ?
N2 Hf P 76.03(5) . . ?
N3 Hf P 170.53(4) . . ?
N3 Hf N1 100.72(6) . . ?
N3 Hf N2 97.20(6) . . ?
N4 Hf P 91.69(5) . . ?
N4 Hf N1 110.63(6) . . ?
N4 Hf N2 121.11(6) . . ?
N4 Hf N3 97.53(6) . . ?
C1 P Hf 104.86(6) . . ?
C1 P C2 103.59(9) . . ?
C2 P Hf 106.85(6) . . ?
C21 P Hf 129.59(6) . . ?
C21 P C1 106.97(9) . . ?
C21 P C2 102.39(9) . . ?
N1 Si1 C9 112.06(8) . . ?
N1 Si1 C10 108.45(9) . . ?
N1 Si1 C11 112.92(8) . . ?
C9 Si1 C10 108.16(10) . . ?
C9 Si1 C11 106.62(10) . . ?
C10 Si1 C11 108.48(10) . . ?
N2 Si2 C18 111.70(9) . . ?
N2 Si2 C19 112.13(9) . . ?
N2 Si2 C20 108.32(8) . . ?
C18 Si2 C19 107.20(10) . . ?
C20 Si2 C18 110.52(11) . . ?
C20 Si2 C19 106.86(10) . . ?
Si1 N1 Hf 129.00(8) . . ?
C4 N1 Hf 118.46(11) . . ?
C4 N1 Si1 112.37(11) . . ?
Si2 N2 Hf 128.23(8) . . ?
C13 N2 Hf 113.60(10) . . ?
C13 N2 Si2 118.03(11) . . ?
C27 N3 Hf 133.27(12) . . ?
C27 N3 C28 110.29(15) . . ?
C28 N3 Hf 116.38(12) . . ?
C29 N4 Hf 124.20(12) . . ?
C29 N4 C30 108.98(15) . . ?
C30 N4 Hf 126.17(12) . . ?
P C1 H1A 110.2 . . ?
P C1 H1B 110.2 . . ?
H1A C1 H1B 108.5 . . ?
C3 C1 P 107.64(12) . . ?
C3 C1 H1A 110.2 . . ?
C3 C1 H1B 110.2 . . ?
P C2 H2A 109.6 . . ?
P C2 H2B 109.6 . . ?
H2A C2 H2B 108.2 . . ?
C12 C2 P 110.11(12) . . ?
C12 C2 H2A 109.6 . . ?
C12 C2 H2B 109.6 . . ?
C4 C3 C1 119.46(15) . . ?
C8 C3 C1 120.85(16) . . ?
C8 C3 C4 119.56(15) . . ?
C3 C4 N1 122.05(14) . . ?
C5 C4 N1 120.07(15) . . ?
C5 C4 C3 117.88(15) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 C4 121.70(17) . . ?
C6 C5 H5 119.2 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 119.99(17) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.11(17) . . ?
C8 C7 H7 120.4 . . ?
C3 C8 H8 119.2 . . ?
C7 C8 C3 121.61(17) . . ?
C7 C8 H8 119.2 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C2 120.75(15) . . ?
C17 C12 C2 119.83(16) . . ?
C17 C12 C13 119.40(16) . . ?
C12 C13 N2 121.78(15) . . ?
C14 C13 N2 120.20(16) . . ?
C14 C13 C12 118.00(16) . . ?
C13 C14 H14 119.1 . . ?
C15 C14 C13 121.82(17) . . ?
C15 C14 H14 119.1 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 119.94(17) . . ?
C16 C15 H15 120.0 . . ?
C15 C16 H16 120.4 . . ?
C15 C16 C17 119.22(17) . . ?
C17 C16 H16 120.4 . . ?
C12 C17 H17 119.2 . . ?
C16 C17 C12 121.60(18) . . ?
C16 C17 H17 119.2 . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si2 C20 H20A 109.5 . . ?
Si2 C20 H20B 109.5 . . ?
Si2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 P 124.84(14) . . ?
C22 C21 C26 118.48(17) . . ?
C26 C21 P 116.64(14) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.78(19) . . ?
C23 C22 H22 119.6 . . ?
C22 C23 H23 119.8 . . ?
C24 C23 C22 120.35(19) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 120.1 . . ?
C23 C24 C25 119.85(19) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 H25 120.1 . . ?
C26 C25 C24 119.9(2) . . ?
C26 C25 H25 120.1 . . ?
C21 C26 H26 119.7 . . ?
C25 C26 C21 120.6(2) . . ?
C25 C26 H26 119.7 . . ?
N3 C27 H27A 109.5 . . ?
N3 C27 H27B 109.5 . . ?
N3 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N3 C28 H28A 109.5 . . ?
N3 C28 H28B 109.5 . . ?
N3 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N4 C29 H29A 109.5 . . ?
N4 C29 H29B 109.5 . . ?
N4 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N4 C30 H30A 109.5 . . ?
N4 C30 H30B 109.5 . . ?
N4 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 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
Hf P C1 C3 -56.70(12) . . . . ?
Hf P C2 C12 -40.42(13) . . . . ?
Hf P C21 C22 135.31(14) . . . . ?
Hf P C21 C26 -46.92(19) . . . . ?
Hf N1 C4 C3 -84.52(17) . . . . ?
Hf N1 C4 C5 95.63(16) . . . . ?
Hf N2 C13 C12 -83.52(16) . . . . ?
Hf N2 C13 C14 94.78(16) . . . . ?
P C1 C3 C4 62.38(18) . . . . ?
P C1 C3 C8 -113.50(16) . . . . ?
P C2 C12 C13 61.85(19) . . . . ?
P C2 C12 C17 -116.58(16) . . . . ?
P C21 C22 C23 177.93(15) . . . . ?
P C21 C26 C25 -176.63(19) . . . . ?
Si1 N1 C4 C3 99.70(16) . . . . ?
Si1 N1 C4 C5 -80.15(17) . . . . ?
Si2 N2 C13 C12 100.55(16) . . . . ?
Si2 N2 C13 C14 -81.14(17) . . . . ?
N1 C4 C5 C6 176.56(16) . . . . ?
N2 C13 C14 C15 -176.51(15) . . . . ?
C1 P C2 C12 70.00(14) . . . . ?
C1 P C21 C22 8.42(18) . . . . ?
C1 P C21 C26 -173.81(15) . . . . ?
C1 C3 C4 N1 8.4(2) . . . . ?
C1 C3 C4 C5 -171.78(15) . . . . ?
C1 C3 C8 C7 174.17(17) . . . . ?
C2 P C1 C3 -168.59(11) . . . . ?
C2 P C21 C22 -100.16(17) . . . . ?
C2 P C21 C26 77.61(17) . . . . ?
C2 C12 C13 N2 -2.2(2) . . . . ?
C2 C12 C13 C14 179.43(15) . . . . ?
C2 C12 C17 C16 179.47(17) . . . . ?
C3 C4 C5 C6 -3.3(3) . . . . ?
C4 C3 C8 C7 -1.7(3) . . . . ?
C4 C5 C6 C7 -0.1(3) . . . . ?
C5 C6 C7 C8 2.7(3) . . . . ?
C6 C7 C8 C3 -1.8(3) . . . . ?
C8 C3 C4 N1 -175.70(15) . . . . ?
C8 C3 C4 C5 4.2(2) . . . . ?
C9 Si1 N1 Hf 0.97(13) . . . . ?
C9 Si1 N1 C4 176.20(12) . . . . ?
C10 Si1 N1 Hf 120.29(11) . . . . ?
C10 Si1 N1 C4 -64.48(13) . . . . ?
C11 Si1 N1 Hf -119.46(11) . . . . ?
C11 Si1 N1 C4 55.77(14) . . . . ?
C12 C13 C14 C15 1.9(2) . . . . ?
C13 C12 C17 C16 1.0(3) . . . . ?
C13 C14 C15 C16 -0.4(3) . . . . ?
C14 C15 C16 C17 -0.8(3) . . . . ?
C15 C16 C17 C12 0.5(3) . . . . ?
C17 C12 C13 N2 176.21(15) . . . . ?
C17 C12 C13 C14 -2.1(2) . . . . ?
C18 Si2 N2 Hf -126.51(11) . . . . ?
C18 Si2 N2 C13 48.74(15) . . . . ?
C19 Si2 N2 Hf 113.12(11) . . . . ?
C19 Si2 N2 C13 -71.63(15) . . . . ?
C20 Si2 N2 Hf -4.56(13) . . . . ?
C20 Si2 N2 C13 170.69(13) . . . . ?
C21 P C1 C3 83.68(13) . . . . ?
C21 P C2 C12 -178.86(12) . . . . ?
C21 C22 C23 C24 -1.1(3) . . . . ?
C22 C21 C26 C25 1.3(3) . . . . ?
C22 C23 C24 C25 0.4(3) . . . . ?
C23 C24 C25 C26 1.1(4) . . . . ?
C24 C25 C26 C21 -1.9(4) . . . . ?
C26 C21 C22 C23 0.2(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            CCD-PXL-KAF2
####################################################################### 
# 
# 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_ba_sb15
_database_code_depnum_ccdc_archive 'CCDC 1440955'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;
_audit_creation_date             2015-12-03

_audit_block_code                ba_sb15
_audit_block_refno               2080
_audit_block_usercomment         sb-mh41


_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C26 H35 Hf I2 N2 P Si2'
_chemical_formula_sum            'C26 H35 Hf I2 N2 P Si2'
_chemical_properties_physical    moisture-sensitive
_chemical_formula_weight         895.00
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      100(1)
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'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/n'
_symmetry_int_tables_number      14

_chemical_absolute_configuration .

_space_group_name_Hall           '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.107(4)
_cell_length_b                   19.914(8)
_cell_length_c                   14.621(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.102(10)
_cell_angle_gamma                90
_cell_volume                     3162(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.22
_cell_measurement_theta_min      2.34
_shelx_estimated_absorpt_T_max   0.614
_shelx_estimated_absorpt_T_min   0.614
_exptl_absorpt_coefficient_mu    5.395
_exptl_absorpt_correction_T_max  0.6179
_exptl_absorpt_correction_T_min  0.5315

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            80926
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.473
_diffrn_reflns_theta_min         2.045
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10080
_reflns_number_total             10886
_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 (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        
'SAINT V8.34A (Bruker AXS, 1997-2013),SADABS-2012_1 (Sheldrick and Bruker AXS, 1997-2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         10886
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0173
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0183P)²+2.2785P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0405
_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:
 C1(H1A,H1B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
I1 I 0.78647(2) 0.75228(2) 0.36884(2) 0.01614(2) Uani 1 1 d . . . . .
I2 I 1.05425(2) 0.61350(2) 0.35810(2) 0.02456(3) Uani 1 1 d . . . . .
Hf Hf 0.82684(2) 0.65206(2) 0.24391(2) 0.01055(2) Uani 1 1 d . . . . .
P P 0.60272(4) 0.69479(2) 0.14167(3) 0.01128(7) Uani 1 1 d . . . . .
Si1 Si 0.75887(4) 0.48228(2) 0.20402(3) 0.01642(9) Uani 1 1 d . . . . .
Si2 Si 0.99297(4) 0.72437(2) 0.10274(3) 0.01721(9) Uani 1 1 d . . . . .
N1 N 0.73319(12) 0.56551(7) 0.23876(9) 0.0132(2) Uani 1 1 d . . . . .
N2 N 0.87571(12) 0.66811(7) 0.11902(9) 0.0131(2) Uani 1 1 d . . . . .
C1 C 0.50270(15) 0.61997(8) 0.13370(11) 0.0152(3) Uani 1 1 d . . . . .
H1A H 0.4162 0.6323 0.1066 0.018 Uiso 1 1 calc R . . . .
H1B H 0.5292 0.5856 0.0931 0.018 Uiso 1 1 calc R . . . .
C2 C 0.51348(15) 0.59286(8) 0.23115(12) 0.0149(3) Uani 1 1 d . . . . .
C3 C 0.62923(15) 0.57221(8) 0.28306(11) 0.0137(3) Uani 1 1 d . . . . .
C4 C 0.64299(17) 0.55749(8) 0.37836(12) 0.0184(3) Uani 1 1 d . . . . .
H4 H 0.7219 0.5460 0.4142 0.022 Uiso 1 1 calc R . . . .
C5 C 0.5428(2) 0.55946(9) 0.42109(14) 0.0243(4) Uani 1 1 d . . . . .
H5 H 0.5532 0.5499 0.4859 0.029 Uiso 1 1 calc R . . . .
C6 C 0.42723(19) 0.57549(10) 0.36879(15) 0.0257(4) Uani 1 1 d . . . . .
H6 H 0.3576 0.5745 0.3971 0.031 Uiso 1 1 calc R . . . .
C7 C 0.41291(16) 0.59300(9) 0.27516(14) 0.0205(3) Uani 1 1 d . . . . .
H7 H 0.3338 0.6052 0.2405 0.025 Uiso 1 1 calc R . . . .
C8 C 0.62814(15) 0.70969(8) 0.02390(11) 0.0145(3) Uani 1 1 d . . . . .
H8A H 0.5477 0.7162 -0.0195 0.017 Uiso 1 1 calc R . . . .
H8B H 0.6766 0.7514 0.0238 0.017 Uiso 1 1 calc R . . . .
C9 C 0.69540(14) 0.65230(8) -0.01032(11) 0.0127(3) Uani 1 1 d . . . . .
C10 C 0.81533(14) 0.63360(8) 0.03549(11) 0.0123(3) Uani 1 1 d . . . . .
C11 C 0.87454(15) 0.58260(8) -0.00381(12) 0.0166(3) Uani 1 1 d . . . . .
H11 H 0.9568 0.5710 0.0246 0.020 Uiso 1 1 calc R . . . .
C12 C 0.81533(16) 0.54852(9) -0.08369(12) 0.0185(3) Uani 1 1 d . . . . .
H12 H 0.8570 0.5135 -0.1086 0.022 Uiso 1 1 calc R . . . .
C13 C 0.69621(16) 0.56528(8) -0.12708(12) 0.0175(3) Uani 1 1 d . . . . .
H13 H 0.6551 0.5415 -0.1809 0.021 Uiso 1 1 calc R . . . .
C14 C 0.63752(15) 0.61754(8) -0.09066(11) 0.0148(3) Uani 1 1 d . . . . .
H14 H 0.5563 0.6299 -0.1210 0.018 Uiso 1 1 calc R . . . .
C15 C 0.50514(14) 0.76429(8) 0.16215(11) 0.0139(3) Uani 1 1 d . . . . .
C16 C 0.47595(17) 0.81632(9) 0.09772(12) 0.0196(3) Uani 1 1 d . . . . .
H16 H 0.5108 0.8171 0.0437 0.023 Uiso 1 1 calc R . . . .
C17 C 0.39587(19) 0.86737(10) 0.11197(13) 0.0248(4) Uani 1 1 d . . . . .
H17 H 0.3765 0.9027 0.0677 0.030 Uiso 1 1 calc R . . . .
C18 C 0.34467(17) 0.86672(10) 0.19032(14) 0.0237(4) Uani 1 1 d . . . . .
H18 H 0.2890 0.9011 0.1993 0.028 Uiso 1 1 calc R . . . .
C19 C 0.37454(17) 0.81588(9) 0.25568(14) 0.0225(3) Uani 1 1 d . . . . .
H19 H 0.3398 0.8157 0.3098 0.027 Uiso 1 1 calc R . . . .
C20 C 0.45517(16) 0.76500(9) 0.24270(12) 0.0181(3) Uani 1 1 d . . . . .
H20 H 0.4764 0.7307 0.2884 0.022 Uiso 1 1 calc R . . . .
C21 C 0.91958(18) 0.47417(10) 0.18836(15) 0.0264(4) Uani 1 1 d . . . . .
H21A H 0.9404 0.5130 0.1536 0.040 Uiso 1 1 calc GR . . . .
H21B H 0.9277 0.4330 0.1535 0.040 Uiso 1 1 calc GR . . . .
H21C H 0.9756 0.4722 0.2498 0.040 Uiso 1 1 calc GR . . . .
C22 C 0.65076(18) 0.46370(9) 0.09107(13) 0.0217(3) Uani 1 1 d . . . . .
H22A H 0.5659 0.4709 0.0981 0.032 Uiso 1 1 calc GR . . . .
H22B H 0.6610 0.4169 0.0734 0.032 Uiso 1 1 calc GR . . . .
H22C H 0.6686 0.4936 0.0423 0.032 Uiso 1 1 calc GR . . . .
C23 C 0.7340(2) 0.42210(9) 0.29564(15) 0.0293(4) Uani 1 1 d . . . . .
H23A H 0.7894 0.4332 0.3552 0.044 Uiso 1 1 calc GR . . . .
H23B H 0.7510 0.3764 0.2771 0.044 Uiso 1 1 calc GR . . . .
H23C H 0.6484 0.4250 0.3029 0.044 Uiso 1 1 calc GR . . . .
C24 C 1.13272(19) 0.67837(12) 0.08613(18) 0.0343(5) Uani 1 1 d . . . . .
H24A H 1.1530 0.6432 0.1337 0.051 Uiso 1 1 calc GR . . . .
H24B H 1.2019 0.7098 0.0922 0.051 Uiso 1 1 calc GR . . . .
H24C H 1.1169 0.6580 0.0238 0.051 Uiso 1 1 calc GR . . . .
C25 C 0.9335(2) 0.77802(12) -0.00078(17) 0.0398(6) Uani 1 1 d . . . . .
H25A H 1.0019 0.8027 -0.0178 0.060 Uiso 1 1 calc GR . . . .
H25B H 0.8732 0.8099 0.0142 0.060 Uiso 1 1 calc GR . . . .
H25C H 0.8939 0.7497 -0.0534 0.060 Uiso 1 1 calc GR . . . .
C26 C 1.03293(19) 0.77961(11) 0.20744(15) 0.0282(4) Uani 1 1 d . . . . .
H26A H 0.9577 0.7998 0.2203 0.042 Uiso 1 1 calc GR . . . .
H26B H 1.0887 0.8152 0.1957 0.042 Uiso 1 1 calc GR . . . .
H26C H 1.0735 0.7530 0.2615 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
I1 Hf 2.8043(8) . ?
I2 Hf 2.8264(8) . ?
Hf P 2.7560(9) . ?
Hf N1 2.0064(15) . ?
Hf N2 2.0363(15) . ?
P C1 1.8477(17) . ?
P C8 1.8267(17) . ?
P C15 1.8208(17) . ?
Si1 N1 1.7740(15) . ?
Si1 C21 1.854(2) . ?
Si1 C22 1.864(2) . ?
Si1 C23 1.861(2) . ?
Si2 N2 1.7714(15) . ?
Si2 C24 1.862(2) . ?
Si2 C25 1.857(2) . ?
Si2 C26 1.862(2) . ?
N1 C3 1.444(2) . ?
N2 C10 1.439(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.505(2) . ?
C2 C3 1.410(2) . ?
C2 C7 1.401(2) . ?
C3 C4 1.400(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.386(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.389(3) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.507(2) . ?
C9 C10 1.410(2) . ?
C9 C14 1.398(2) . ?
C10 C11 1.397(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.391(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.383(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.392(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.392(2) . ?
C15 C20 1.403(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.395(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.382(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.384(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.391(2) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 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
I1 Hf I2 93.08(2) . . ?
P Hf I1 83.33(2) . . ?
P Hf I2 176.376(9) . . ?
N1 Hf I1 118.91(4) . . ?
N1 Hf I2 100.42(4) . . ?
N1 Hf P 80.95(4) . . ?
N1 Hf N2 109.56(6) . . ?
N2 Hf I1 125.55(4) . . ?
N2 Hf I2 101.49(5) . . ?
N2 Hf P 81.11(5) . . ?
C1 P Hf 104.36(6) . . ?
C8 P Hf 105.12(6) . . ?
C8 P C1 106.33(8) . . ?
C15 P Hf 130.29(5) . . ?
C15 P C1 104.63(8) . . ?
C15 P C8 104.27(8) . . ?
N1 Si1 C21 109.48(8) . . ?
N1 Si1 C22 109.07(7) . . ?
N1 Si1 C23 109.79(8) . . ?
C21 Si1 C22 109.35(9) . . ?
C21 Si1 C23 108.97(10) . . ?
C23 Si1 C22 110.16(10) . . ?
N2 Si2 C24 111.28(9) . . ?
N2 Si2 C25 109.10(9) . . ?
N2 Si2 C26 108.57(8) . . ?
C25 Si2 C24 109.92(12) . . ?
C25 Si2 C26 108.24(12) . . ?
C26 Si2 C24 109.66(11) . . ?
Si1 N1 Hf 134.44(8) . . ?
C3 N1 Hf 111.15(10) . . ?
C3 N1 Si1 113.99(10) . . ?
Si2 N2 Hf 124.16(7) . . ?
C10 N2 Hf 121.44(10) . . ?
C10 N2 Si2 114.40(10) . . ?
P C1 H1A 110.2 . . ?
P C1 H1B 110.2 . . ?
H1A C1 H1B 108.5 . . ?
C2 C1 P 107.58(11) . . ?
C2 C1 H1A 110.2 . . ?
C2 C1 H1B 110.2 . . ?
C3 C2 C1 119.79(14) . . ?
C7 C2 C1 121.42(16) . . ?
C7 C2 C3 118.55(16) . . ?
C2 C3 N1 120.67(14) . . ?
C4 C3 N1 119.76(15) . . ?
C4 C3 C2 119.57(15) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.79(17) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.71(18) . . ?
C6 C5 H5 120.1 . . ?
C5 C6 H6 119.9 . . ?
C5 C6 C7 120.19(17) . . ?
C7 C6 H6 119.9 . . ?
C2 C7 H7 119.5 . . ?
C6 C7 C2 120.97(18) . . ?
C6 C7 H7 119.5 . . ?
P C8 H8A 109.2 . . ?
P C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C9 C8 P 112.03(11) . . ?
C9 C8 H8A 109.2 . . ?
C9 C8 H8B 109.2 . . ?
C10 C9 C8 121.82(14) . . ?
C14 C9 C8 118.79(14) . . ?
C14 C9 C10 119.38(14) . . ?
C9 C10 N2 120.20(14) . . ?
C11 C10 N2 121.36(14) . . ?
C11 C10 C9 118.41(15) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 C10 121.30(16) . . ?
C12 C11 H11 119.4 . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.39(15) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 120.5 . . ?
C12 C13 C14 119.00(15) . . ?
C14 C13 H13 120.5 . . ?
C9 C14 H14 119.3 . . ?
C13 C14 C9 121.45(15) . . ?
C13 C14 H14 119.3 . . ?
C16 C15 P 121.11(13) . . ?
C16 C15 C20 118.90(15) . . ?
C20 C15 P 119.96(13) . . ?
C15 C16 H16 119.8 . . ?
C15 C16 C17 120.45(17) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 119.9 . . ?
C18 C17 C16 120.21(18) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 119.90(17) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 119.8 . . ?
C18 C19 C20 120.43(17) . . ?
C20 C19 H19 119.8 . . ?
C15 C20 H20 120.0 . . ?
C19 C20 C15 120.07(17) . . ?
C19 C20 H20 120.0 . . ?
Si1 C21 H21A 109.5 . . ?
Si1 C21 H21B 109.5 . . ?
Si1 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si1 C22 H22A 109.5 . . ?
Si1 C22 H22B 109.5 . . ?
Si1 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si2 C25 H25A 109.5 . . ?
Si2 C25 H25B 109.5 . . ?
Si2 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 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
Hf P C1 C2 50.87(11) . . . . ?
Hf P C8 C9 47.35(12) . . . . ?
Hf P C15 C16 119.19(13) . . . . ?
Hf P C15 C20 -62.63(16) . . . . ?
Hf N1 C3 C2 89.48(15) . . . . ?
Hf N1 C3 C4 -91.12(15) . . . . ?
Hf N2 C10 C9 74.44(17) . . . . ?
Hf N2 C10 C11 -107.58(15) . . . . ?
P C1 C2 C3 -59.73(17) . . . . ?
P C1 C2 C7 114.60(15) . . . . ?
P C8 C9 C10 -61.88(18) . . . . ?
P C8 C9 C14 119.18(14) . . . . ?
P C15 C16 C17 176.60(14) . . . . ?
P C15 C20 C19 -176.04(14) . . . . ?
Si1 N1 C3 C2 -96.88(15) . . . . ?
Si1 N1 C3 C4 82.52(16) . . . . ?
Si2 N2 C10 C9 -105.43(14) . . . . ?
Si2 N2 C10 C11 72.55(17) . . . . ?
N1 C3 C4 C5 -175.91(15) . . . . ?
N2 C10 C11 C12 178.93(15) . . . . ?
C1 P C8 C9 -62.94(13) . . . . ?
C1 P C15 C16 -116.94(15) . . . . ?
C1 P C15 C20 61.23(15) . . . . ?
C1 C2 C3 N1 -11.0(2) . . . . ?
C1 C2 C3 C4 169.59(14) . . . . ?
C1 C2 C7 C6 -172.16(16) . . . . ?
C2 C3 C4 C5 3.5(2) . . . . ?
C3 C2 C7 C6 2.2(2) . . . . ?
C3 C4 C5 C6 0.7(3) . . . . ?
C4 C5 C6 C7 -3.4(3) . . . . ?
C5 C6 C7 C2 1.9(3) . . . . ?
C7 C2 C3 N1 174.50(14) . . . . ?
C7 C2 C3 C4 -4.9(2) . . . . ?
C8 P C1 C2 161.71(11) . . . . ?
C8 P C15 C16 -5.46(16) . . . . ?
C8 P C15 C20 172.72(13) . . . . ?
C8 C9 C10 N2 2.0(2) . . . . ?
C8 C9 C10 C11 -176.06(15) . . . . ?
C8 C9 C14 C13 178.25(15) . . . . ?
C9 C10 C11 C12 -3.1(2) . . . . ?
C10 C9 C14 C13 -0.7(2) . . . . ?
C10 C11 C12 C13 1.0(3) . . . . ?
C11 C12 C13 C14 1.2(2) . . . . ?
C12 C13 C14 C9 -1.4(2) . . . . ?
C14 C9 C10 N2 -179.09(14) . . . . ?
C14 C9 C10 C11 2.9(2) . . . . ?
C15 P C1 C2 -88.30(12) . . . . ?
C15 P C8 C9 -173.19(11) . . . . ?
C15 C16 C17 C18 0.0(3) . . . . ?
C16 C15 C20 C19 2.2(3) . . . . ?
C16 C17 C18 C19 1.1(3) . . . . ?
C17 C18 C19 C20 -0.5(3) . . . . ?
C18 C19 C20 C15 -1.1(3) . . . . ?
C20 C15 C16 C17 -1.6(3) . . . . ?
C21 Si1 N1 Hf 11.69(14) . . . . ?
C21 Si1 N1 C3 -159.99(12) . . . . ?
C22 Si1 N1 Hf -107.92(12) . . . . ?
C22 Si1 N1 C3 80.39(13) . . . . ?
C23 Si1 N1 Hf 131.29(12) . . . . ?
C23 Si1 N1 C3 -40.40(14) . . . . ?
C24 Si2 N2 Hf 106.75(11) . . . . ?
C24 Si2 N2 C10 -73.38(14) . . . . ?
C25 Si2 N2 Hf -131.79(12) . . . . ?
C25 Si2 N2 C10 48.07(15) . . . . ?
C26 Si2 N2 Hf -14.03(12) . . . . ?
C26 Si2 N2 C10 165.83(12) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            CCD-PXL-KAF2
####################################################################### 
# 
# 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_ba_tk4_4
_database_code_depnum_ccdc_archive 'CCDC 1440956'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;
_audit_creation_date             
;
'Mon Mar 02 18:39:36 2015'
;

_audit_block_code                ba_tk4
_audit_block_refno               2354
_audit_block_usercomment         'TK102, plate, red'


_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C24 H35 Cl2 N2 P Ti'
_chemical_formula_sum            'C24 H35 Cl2 N2 P Ti'
_chemical_properties_physical    moisture-sensitive
_chemical_formula_weight         501.31
_chemical_melting_point          ?
_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_diffrn_ambient_temperature      120(1)
_chemical_oxdiff_formula         'C24 H35 Cl2 N2 P Ti'
_chemical_oxdiff_usercomment     'TK102, plate, red'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 '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'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_h-m   'P n m a'
_symmetry_int_tables_number      62
_chemical_absolute_configuration .

_space_group_name_Hall           '-P 2ac 2n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   13.8960(3)
_cell_length_b                   20.0990(4)
_cell_length_c                   9.01231(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2517.10(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    18276
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.6330
_cell_measurement_theta_min      5.3660
_shelx_estimated_absorpt_T_max   0.608
_shelx_estimated_absorpt_T_min   0.072
_exptl_absorpt_coefficient_mu    5.528
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.036
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1029
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            39026
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.048
_diffrn_reflns_theta_min         5.852
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   10.00   38.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -30.0000 28

#__ type_ start__ end____ width___ exp.time_
  2 omega  -20.00   66.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 86

#__ type_ start__ end____ width___ exp.time_
  3 omega  -59.00    1.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   60.0000 60

#__ type_ start__ end____ width___ exp.time_
  4 omega   41.00   72.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -30.0000 31

#__ type_ start__ end____ width___ exp.time_
  5 omega  -25.00    7.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -30.0000 32

#__ type_ start__ end____ width___ exp.time_
  6 omega  -69.00   21.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -180.0000 90

#__ type_ start__ end____ width___ exp.time_
  7 omega   24.00   54.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 30

#__ type_ start__ end____ width___ exp.time_
  8 omega    3.00   73.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000  -90.0000 70

#__ type_ start__ end____ width___ exp.time_
  9 omega   24.00   50.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 10 omega   -9.00   74.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -60.0000 83

#__ type_ start__ end____ width___ exp.time_
 11 omega   24.00   67.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 43

#__ type_ start__ end____ width___ exp.time_
 12 omega   24.00   50.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 13 omega   75.00  119.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -180.0000 44

#__ type_ start__ end____ width___ exp.time_
 14 omega   62.00  122.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 60

#__ type_ start__ end____ width___ exp.time_
 15 omega   24.00   62.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 38

#__ type_ start__ end____ width___ exp.time_
 16 omega   81.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 43

#__ type_ start__ end____ width___ exp.time_
 17 omega   23.00   94.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000  120.0000 71

#__ type_ start__ end____ width___ exp.time_
 18 omega   25.00   68.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -180.0000 43

#__ type_ start__ end____ width___ exp.time_
 19 omega   24.00   56.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 32

#__ type_ start__ end____ width___ exp.time_
 20 omega   24.00  120.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 96

#__ type_ start__ end____ width___ exp.time_
 21 omega   87.00  122.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 35

#__ type_ start__ end____ width___ exp.time_
 22 omega  -14.00   72.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  120.0000 86

#__ type_ start__ end____ width___ exp.time_
 23 omega   55.00  108.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 53

#__ type_ start__ end____ width___ exp.time_
 24 omega   24.00   58.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 34

#__ type_ start__ end____ width___ exp.time_
 25 omega   26.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 98

#__ type_ start__ end____ width___ exp.time_
 26 omega   57.00  112.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 55

#__ type_ start__ end____ width___ exp.time_
 27 omega   24.00   51.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
 28 omega   24.00   53.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 29

#__ type_ start__ end____ width___ exp.time_
 29 omega   80.00  118.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 38

#__ type_ start__ end____ width___ exp.time_
 30 omega   82.00  157.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  120.0000 75

#__ type_ start__ end____ width___ exp.time_
 31 omega   45.00   72.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 27

#__ type_ start__ end____ width___ exp.time_
 32 omega   78.00  162.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 84

#__ type_ start__ end____ width___ exp.time_
 33 omega   85.00  133.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 48

#__ type_ start__ end____ width___ exp.time_
 34 omega   85.00  111.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 35 omega   80.00  106.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000  135.2122 26

#__ type_ start__ end____ width___ exp.time_
 36 omega  117.00  144.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000  -76.5469 27

#__ type_ start__ end____ width___ exp.time_
 37 omega   78.00  104.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 38 omega   78.00  123.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 45

#__ type_ start__ end____ width___ exp.time_
 39 omega   80.00  177.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000   14.0621 97

#__ type_ start__ end____ width___ exp.time_
 40 omega   36.00  125.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000 -180.0000 89

#__ type_ start__ end____ width___ exp.time_
 41 omega   78.00  104.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 42 omega  117.00  144.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   73.0000 -137.3822 27

#__ type_ start__ end____ width___ exp.time_
 43 omega   79.00  105.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000  -76.5469 26

#__ type_ start__ end____ width___ exp.time_
 44 omega   80.00  156.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000  -50.0831 76

#__ type_ start__ end____ width___ exp.time_
 45 omega   78.00  176.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 98

#__ type_ start__ end____ width___ exp.time_
 46 omega   80.00  107.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   73.0000 -137.3822 27

#__ type_ start__ end____ width___ exp.time_
 47 omega   78.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 100

#__ type_ start__ end____ width___ exp.time_
 48 omega   78.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 100

#__ type_ start__ end____ width___ exp.time_
 49 omega   78.00  139.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 61

#__ type_ start__ end____ width___ exp.time_
 50 omega   37.00  120.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000    0.0000 83

#__ type_ start__ end____ width___ exp.time_
 51 omega  118.00  175.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   58.0000   86.1952 57

#__ type_ start__ end____ width___ exp.time_
 52 omega   79.00  172.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000 -162.6481 93

#__ type_ start__ end____ width___ exp.time_
 53 omega   78.00  111.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 33

#__ type_ start__ end____ width___ exp.time_
 54 omega   79.00  104.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
 55 omega   79.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 99

#__ type_ start__ end____ width___ exp.time_
 56 omega   88.00  113.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   58.0000   86.1952 25

#__ type_ start__ end____ width___ exp.time_
 57 omega   57.00  111.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  150.0000 54

#__ type_ start__ end____ width___ exp.time_
 58 omega   78.00  104.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 59 omega   85.00  111.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 60 omega   85.00  111.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
 61 omega   79.00  105.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000  166.7059 26

#__ type_ start__ end____ width___ exp.time_
 62 omega   85.00  118.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 33

#__ type_ start__ end____ width___ exp.time_
 63 omega   79.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000   40.2016 99

#__ type_ start__ end____ width___ exp.time_
 64 omega  151.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  106.6256 27

#__ type_ start__ end____ width___ exp.time_
 65 omega   39.00  103.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000    0.0000 64

#__ type_ start__ end____ width___ exp.time_
 66 omega   37.00  116.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -30.0000 79

#__ type_ start__ end____ width___ exp.time_
 67 omega   78.00  104.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  106.6256 26

#__ type_ start__ end____ width___ exp.time_
 68 omega  -69.00   21.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 90

#__ type_ start__ end____ width___ exp.time_
 69 omega  -70.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000 -120.0000 100

#__ type_ start__ end____ width___ exp.time_
 70 omega  -54.00    2.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  120.0000 -138.0000 56

#__ type_ start__ end____ width___ exp.time_
 71 omega  -21.00   69.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  120.0000 90

#__ type_ start__ end____ width___ exp.time_
 72 omega  -69.00   21.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -60.0000 90

#__ type_ start__ end____ width___ exp.time_
 73 omega    1.00   96.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000  120.0000 95

#__ type_ start__ end____ width___ exp.time_
 74 omega   28.00  126.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000   60.0000 98

#__ type_ start__ end____ width___ exp.time_
 75 omega  -18.00   80.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000  120.0000 98

#__ type_ start__ end____ width___ exp.time_
 76 omega  -16.00   84.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000  -90.0000 100

#__ type_ start__ end____ width___ exp.time_
 77 omega   33.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -150.0000 90

#__ type_ start__ end____ width___ exp.time_
 78 omega   33.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -30.0000 90

#__ type_ start__ end____ width___ exp.time_
 79 omega   33.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -90.0000 90

#__ type_ start__ end____ width___ exp.time_
 80 omega   33.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  150.0000 90

#__ type_ start__ end____ width___ exp.time_
 81 omega   33.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  120.0000 90

#__ type_ start__ end____ width___ exp.time_
 82 omega   24.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 100

#__ type_ start__ end____ width___ exp.time_
 83 omega    1.00   96.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000  -60.0000 95

#__ type_ start__ end____ width___ exp.time_
 84 omega   33.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -180.0000 90

#__ type_ start__ end____ width___ exp.time_
 85 omega   24.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 100

#__ type_ start__ end____ width___ exp.time_
 86 omega    1.00   96.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000   60.0000 95

#__ type_ start__ end____ width___ exp.time_
 87 omega   24.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 100

#__ type_ start__ end____ width___ exp.time_
 88 omega   19.00  108.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -120.0000  137.0000 89

#__ type_ start__ end____ width___ exp.time_
 89 omega   33.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -60.0000 90

#__ type_ start__ end____ width___ exp.time_
 90 omega   24.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 100

#__ type_ start__ end____ width___ exp.time_
 91 omega   28.00  126.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000 -180.0000 98

#__ type_ start__ end____ width___ exp.time_
 92 omega   24.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 100

#__ type_ start__ end____ width___ exp.time_
 93 omega   36.00   93.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -30.0000 57

#__ type_ start__ end____ width___ exp.time_
 94 omega  100.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -120.0000 78

#__ type_ start__ end____ width___ exp.time_
 95 omega   36.00   93.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -150.0000 57

#__ type_ start__ end____ width___ exp.time_
 96 omega   35.00   94.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   90.0000 59

#__ type_ start__ end____ width___ exp.time_
 97 omega   36.00  116.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 80

#__ type_ start__ end____ width___ exp.time_
 98 omega   35.00   94.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  150.0000 59

#__ type_ start__ end____ width___ exp.time_
 99 omega  100.00  145.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  150.0000 45

#__ type_ start__ end____ width___ exp.time_
100 omega   36.00  146.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000  150.0000 110

#__ type_ start__ end____ width___ exp.time_
101 omega   78.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 100

#__ type_ start__ end____ width___ exp.time_
102 omega   86.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  -90.0000 92

#__ type_ start__ end____ width___ exp.time_
103 omega   86.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000   60.0000 92

#__ type_ start__ end____ width___ exp.time_
104 omega   79.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000 -162.6481 99

#__ type_ start__ end____ width___ exp.time_
105 omega   35.00   94.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -90.0000 59

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0134927000
_diffrn_orient_matrix_UB_12      -0.0760591000
_diffrn_orient_matrix_UB_13      -0.0017524000
_diffrn_orient_matrix_UB_21      0.0123083000
_diffrn_orient_matrix_UB_22      0.0002962000
_diffrn_orient_matrix_UB_23      0.1699014000
_diffrn_orient_matrix_UB_31      -0.1093605000
_diffrn_orient_matrix_UB_32      -0.0093537000
_diffrn_orient_matrix_UB_33      0.0189036000
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.7769 9031 56625
2 0.2231 0 56625
_diffrn_oxdiff_twin_integration_method simultaneous
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2144
_reflns_number_total             2452
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.328
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2452
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0890
_refine_ls_restrained_S_all      1.328
_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)+16.1905P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.1932
_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: H1A(0.5) H1B(0.5)
3.a Ternary CH refined with riding coordinates:
 C2(H2)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16)
3.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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 0.20952(10) 0.7500 0.66598(17) 0.0260(4) Uani 1 2 d S T P . .
Cl1 Cl 0.27044(15) 0.7500 0.9144(2) 0.0331(5) Uani 1 2 d S T P . .
Cl2 Cl 0.05191(17) 0.7500 0.7532(3) 0.0837(13) Uani 1 2 d S T P . .
P P 0.14623(15) 0.7500 0.3949(2) 0.0329(6) Uani 1 2 d S T P . .
N1 N 0.2764(3) 0.6755(2) 0.5978(5) 0.0285(11) Uani 1 1 d . . . . .
C1 C 0.2643(6) 0.7500 0.3004(10) 0.045(3) Uani 1 2 d S T P . .
H1A H 0.2684 0.7102 0.2359 0.054 Uiso 0.5 1 calc R . . . .
H1B H 0.2684 0.7898 0.2359 0.054 Uiso 0.5 1 calc R . . . .
C2 C 0.3507(5) 0.7500 0.4063(9) 0.0224(16) Uani 1 2 d S T P . .
H2 H 0.4087 0.7500 0.3407 0.027 Uiso 1 2 calc RS T P . .
C4 C 0.3575(4) 0.6863(3) 0.4959(7) 0.0324(14) Uani 1 1 d . . . . .
H4A H 0.3615 0.6482 0.4266 0.039 Uiso 1 1 calc R . . . .
H4B H 0.4179 0.6873 0.5543 0.039 Uiso 1 1 calc R . . . .
C11 C 0.0818(4) 0.6782(3) 0.3218(7) 0.0339(14) Uani 1 1 d . . . . .
C12 C 0.0102(5) 0.6496(5) 0.4099(9) 0.068(3) Uani 1 1 d . . . . .
H12 H -0.0069 0.6696 0.5017 0.082 Uiso 1 1 calc R . . . .
C13 C -0.0360(6) 0.5922(6) 0.3640(10) 0.074(3) Uani 1 1 d . . . . .
H13 H -0.0846 0.5732 0.4248 0.088 Uiso 1 1 calc R . . . .
C14 C -0.0127(5) 0.5622(4) 0.2324(11) 0.054(2) Uani 1 1 d . . . . .
H14 H -0.0432 0.5220 0.2032 0.065 Uiso 1 1 calc R . . . .
C15 C 0.0554(5) 0.5913(3) 0.1436(10) 0.050(2) Uani 1 1 d . . . . .
H15 H 0.0709 0.5714 0.0510 0.060 Uiso 1 1 calc R . . . .
C16 C 0.1018(5) 0.6488(3) 0.1858(8) 0.0364(15) Uani 1 1 d . . . . .
H16 H 0.1478 0.6685 0.1215 0.044 Uiso 1 1 calc R . . . .
C21 C 0.2682(5) 0.6055(3) 0.6527(8) 0.0432(17) Uani 1 1 d . . . . .
C22 C 0.2544(6) 0.5571(3) 0.5231(9) 0.051(2) Uani 1 1 d . . . . .
H22A H 0.1975 0.5701 0.4657 0.077 Uiso 1 1 calc GR . . . .
H22B H 0.2455 0.5119 0.5617 0.077 Uiso 1 1 calc GR . . . .
H22C H 0.3113 0.5583 0.4590 0.077 Uiso 1 1 calc GR . . . .
C23 C 0.3602(7) 0.5887(3) 0.7390(10) 0.066(3) Uani 1 1 d . . . . .
H23A H 0.4161 0.5939 0.6739 0.100 Uiso 1 1 calc GR . . . .
H23B H 0.3568 0.5426 0.7742 0.100 Uiso 1 1 calc GR . . . .
H23C H 0.3663 0.6187 0.8241 0.100 Uiso 1 1 calc GR . . . .
C24 C 0.1810(7) 0.5999(4) 0.7547(9) 0.071(3) Uani 1 1 d . . . . .
H24A H 0.1880 0.6310 0.8378 0.106 Uiso 1 1 calc GR . . . .
H24B H 0.1763 0.5544 0.7930 0.106 Uiso 1 1 calc GR . . . .
H24C H 0.1225 0.6107 0.6989 0.106 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 Cl1 2.394(2) . ?
Ti Cl2 2.327(3) . ?
Ti P 2.597(3) . ?
Ti N1 1.867(5) 8_575 ?
Ti N1 1.867(5) . ?
P C1 1.848(9) . ?
P C11 1.821(7) 8_575 ?
P C11 1.821(7) . ?
N1 C4 1.471(7) . ?
N1 C21 1.495(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.533(11) . ?
C2 H2 1.0000 . ?
C2 C4 1.516(7) . ?
C2 C4 1.516(7) 8_575 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C11 C12 1.397(9) . ?
C11 C16 1.388(9) . ?
C12 H12 0.9500 . ?
C12 C13 1.384(13) . ?
C13 H13 0.9500 . ?
C13 C14 1.369(13) . ?
C14 H14 0.9500 . ?
C14 C15 1.371(10) . ?
C15 H15 0.9500 . ?
C15 C16 1.378(9) . ?
C16 H16 0.9500 . ?
C21 C22 1.533(9) . ?
C21 C23 1.534(10) . ?
C21 C24 1.526(11) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
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
Cl1 Ti P 179.09(9) . . ?
Cl2 Ti Cl1 90.96(10) . . ?
Cl2 Ti P 89.95(10) . . ?
N1 Ti Cl1 97.59(16) 8_575 . ?
N1 Ti Cl1 97.59(16) . . ?
N1 Ti Cl2 125.41(14) . . ?
N1 Ti Cl2 125.42(14) 8_575 . ?
N1 Ti P 81.88(16) . . ?
N1 Ti P 81.88(16) 8_575 . ?
N1 Ti N1 106.7(3) 8_575 . ?
C1 P Ti 97.6(3) . . ?
C11 P Ti 120.5(2) . . ?
C11 P Ti 120.5(2) 8_575 . ?
C11 P C1 105.6(3) 8_575 . ?
C11 P C1 105.6(3) . . ?
C11 P C11 104.7(4) . 8_575 ?
C4 N1 Ti 117.9(4) . . ?
C4 N1 C21 113.9(5) . . ?
C21 N1 Ti 127.4(4) . . ?
P C1 H1A 108.7 . . ?
P C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C2 C1 P 114.1(6) . . ?
C2 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
C1 C2 H2 105.3 . . ?
C4 C2 C1 112.4(4) . . ?
C4 C2 C1 112.4(4) 8_575 . ?
C4 C2 H2 105.3 . . ?
C4 C2 H2 105.3 8_575 . ?
C4 C2 C4 115.1(7) . 8_575 ?
N1 C4 C2 114.2(5) . . ?
N1 C4 H4A 108.7 . . ?
N1 C4 H4B 108.7 . . ?
C2 C4 H4A 108.7 . . ?
C2 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C12 C11 P 118.1(6) . . ?
C16 C11 P 123.9(5) . . ?
C16 C11 C12 118.0(7) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.2(8) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 119.4 . . ?
C14 C13 C12 121.1(7) . . ?
C14 C13 H13 119.4 . . ?
C13 C14 H14 120.6 . . ?
C13 C14 C15 118.8(8) . . ?
C15 C14 H14 120.6 . . ?
C14 C15 H15 119.3 . . ?
C14 C15 C16 121.3(8) . . ?
C16 C15 H15 119.3 . . ?
C11 C16 H16 119.7 . . ?
C15 C16 C11 120.5(6) . . ?
C15 C16 H16 119.7 . . ?
N1 C21 C22 110.7(5) . . ?
N1 C21 C23 108.2(5) . . ?
N1 C21 C24 109.2(6) . . ?
C22 C21 C23 110.5(7) . . ?
C24 C21 C22 108.2(6) . . ?
C24 C21 C23 109.9(7) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 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
Ti P C1 C2 0.000(1) . . . . ?
Ti P C11 C12 45.6(6) . . . . ?
Ti P C11 C16 -132.1(5) . . . . ?
Ti N1 C4 C2 -26.0(7) . . . . ?
Ti N1 C21 C22 130.6(6) . . . . ?
Ti N1 C21 C23 -108.1(7) . . . . ?
Ti N1 C21 C24 11.5(8) . . . . ?
Cl1 Ti N1 C4 -106.6(4) . . . . ?
Cl1 Ti N1 C21 62.5(5) . . . . ?
Cl2 Ti N1 C4 156.7(4) . . . . ?
Cl2 Ti N1 C21 -34.1(6) . . . . ?
P Ti N1 C4 72.6(4) . . . . ?
P Ti N1 C21 -118.3(5) . . . . ?
P C1 C2 C4 65.9(5) . . . . ?
P C1 C2 C4 -65.9(5) . . . 8_575 ?
P C11 C12 C13 -175.3(7) . . . . ?
P C11 C16 C15 174.5(5) . . . . ?
N1 Ti N1 C4 -6.3(6) 8_575 . . . ?
N1 Ti N1 C21 162.8(4) 8_575 . . . ?
C1 P C11 C12 154.5(6) . . . . ?
C1 P C11 C16 -23.2(6) . . . . ?
C1 C2 C4 N1 -64.1(7) . . . . ?
C4 N1 C21 C22 -59.9(7) . . . . ?
C4 N1 C21 C23 61.4(8) . . . . ?
C4 N1 C21 C24 -179.0(6) . . . . ?
C4 C2 C4 N1 66.2(9) 8_575 . . . ?
C11 P C1 C2 124.7(2) 8_575 . . . ?
C11 P C1 C2 -124.7(2) . . . . ?
C11 P C11 C12 -94.2(6) 8_575 . . . ?
C11 P C11 C16 88.2(6) 8_575 . . . ?
C11 C12 C13 C14 0.1(13) . . . . ?
C12 C11 C16 C15 -3.2(10) . . . . ?
C12 C13 C14 C15 -2.1(13) . . . . ?
C13 C14 C15 C16 1.4(12) . . . . ?
C14 C15 C16 C11 1.2(11) . . . . ?
C16 C11 C12 C13 2.5(11) . . . . ?
C21 N1 C4 C2 163.5(5) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
8 2 -2 0.0355 8.0023 1.9912 -2.0007 -0.0400 -0.2408 -0.9316
-9 -1 -1 0.0309 -9.0037 -0.9934 -0.9981 -0.0442 -0.2807 0.9751
-3 0 -5 0.0481 -3.0030 -0.0026 -4.9975 -0.0316 -0.8861 0.2340
-8 -2 2 0.0355 -8.0023 -1.9912 2.0007 0.0400 0.2408 0.9316
2 -13 0 0.0179 1.9991 -13.0033 0.0024 1.0160 0.0212 -0.0969
-2 13 0 0.0179 -1.9991 13.0033 -0.0024 -1.0160 -0.0212 0.0969
-8 -1 2 0.0281 -8.0022 -0.9911 2.0005 -0.0361 0.2411 0.9222
3 0 5 0.0481 3.0030 0.0026 4.9975 0.0316 0.8861 -0.2340

_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            13.8946(4)
_cell_oxdiff_length_b            20.1031(4)
_cell_oxdiff_length_c            9.01134(16)
_cell_oxdiff_angle_alpha         90.0295(16)
_cell_oxdiff_angle_beta          90.0004(19)
_cell_oxdiff_angle_gamma         90.002(2)
_cell_oxdiff_volume              2517.10(10)
_cell_oxdiff_measurement_reflns_used 17913
_cell_oxdiff_twin_number         2
loop_
_twin_individual_id
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 -0.9996 0.0171 -0.0010 -0.0438 -0.9992 -0.0026 -0.0004 -0.0006 1.0001
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ba_tk6
_database_code_depnum_ccdc_archive 'CCDC 1440957'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;
_audit_creation_date             2015-12-03

_audit_block_code                ba_tk6
_audit_block_refno               2462
_audit_block_usercomment         TK174


_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C24 H35 Cl2 Hf N2 P'
_chemical_formula_sum            'C24 H35 Cl2 Hf N2 P'
_chemical_properties_physical    moisture-sensitive
_chemical_formula_weight         631.90
_chemical_melting_point          ?
_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      100(1)
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'
Hf Hf -0.5830 6.1852 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14

_chemical_absolute_configuration .

_space_group_name_Hall           '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.516(4)
_cell_length_b                   29.311(11)
_cell_length_c                   9.277(4)
_cell_angle_alpha                90
_cell_angle_beta                 114.210(9)
_cell_angle_gamma                90
_cell_volume                     2608.0(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8183
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.45
_cell_measurement_theta_min      2.23
_shelx_estimated_absorpt_T_max   0.606
_shelx_estimated_absorpt_T_min   0.380
_exptl_absorpt_coefficient_mu    4.280
_exptl_absorpt_correction_T_max  0.4348
_exptl_absorpt_correction_T_min  0.3284

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            38967
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.389
_diffrn_detector_area_resol_mean 8.19
_diffrn_detector_type            CCD-PXL-KAF2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4534
_reflns_number_total             4605
_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 (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        
'SAINT V8.34A (Bruker AXS, 1997-2013),SADABS-2014_5 (Sheldrick and Bruker AXS, 1997-2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         1.322
_refine_diff_density_min         -2.378
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.426
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4605
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0330
_refine_ls_restrained_S_all      1.426
_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)+15.5919P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0705
_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 Ternary CH refined with riding coordinates:
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
2.c 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)
2.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
Hf Hf 0.31924(2) 0.63656(2) -0.03211(2) 0.00983(7) Uani 1 1 d . . . . .
Cl1 Cl 0.33449(13) 0.66599(4) -0.27398(14) 0.0157(3) Uani 1 1 d . . . . .
Cl2 Cl 0.31376(14) 0.55740(4) -0.11488(15) 0.0185(3) Uani 1 1 d . . . . .
P P 0.31238(14) 0.60973(4) 0.24584(15) 0.0113(3) Uani 1 1 d . . . . .
N1 N 0.4780(5) 0.67187(15) 0.1249(5) 0.0145(9) Uani 1 1 d . . . . .
N2 N 0.1547(5) 0.67307(14) -0.0434(5) 0.0134(9) Uani 1 1 d . . . . .
C1 C 0.3104(5) 0.70755(17) 0.2234(6) 0.0138(11) Uani 1 1 d . . . . .
H1 H 0.3081 0.7352 0.2852 0.017 Uiso 1 1 calc R . . . .
C2 C 0.3113(6) 0.66726(18) 0.3288(6) 0.0182(12) Uani 1 1 d . . . . .
H2A H 0.2282 0.6697 0.3529 0.022 Uiso 1 1 calc R . . . .
H2B H 0.3945 0.6700 0.4300 0.022 Uiso 1 1 calc R . . . .
C3 C 0.4447(6) 0.7120(2) 0.2000(7) 0.0237(13) Uani 1 1 d . . . . .
H3A H 0.4377 0.7392 0.1339 0.028 Uiso 1 1 calc R . . . .
H3B H 0.5227 0.7172 0.3042 0.028 Uiso 1 1 calc R . . . .
C4 C 0.1763(6) 0.7105(2) 0.0701(6) 0.0222(13) Uani 1 1 d . . . . .
H4A H 0.0954 0.7114 0.0989 0.027 Uiso 1 1 calc R . . . .
H4B H 0.1774 0.7397 0.0168 0.027 Uiso 1 1 calc R . . . .
C5 C 0.1637(5) 0.58074(17) 0.2606(6) 0.0127(10) Uani 1 1 d . . . . .
C6 C 0.1480(6) 0.57963(18) 0.4027(7) 0.0182(12) Uani 1 1 d . . . . .
H6 H 0.2148 0.5939 0.4943 0.022 Uiso 1 1 calc R . . . .
C7 C 0.0338(6) 0.55741(19) 0.4092(7) 0.0204(12) Uani 1 1 d . . . . .
H7 H 0.0223 0.5568 0.5056 0.024 Uiso 1 1 calc R . . . .
C8 C -0.0635(6) 0.53608(19) 0.2767(7) 0.0205(12) Uani 1 1 d . . . . .
H8 H -0.1411 0.5208 0.2821 0.025 Uiso 1 1 calc R . . . .
C9 C -0.0467(6) 0.53721(19) 0.1365(7) 0.0213(12) Uani 1 1 d . . . . .
H9 H -0.1136 0.5227 0.0453 0.026 Uiso 1 1 calc R . . . .
C10 C 0.0659(6) 0.55915(19) 0.1275(6) 0.0180(12) Uani 1 1 d . . . . .
H10 H 0.0767 0.5595 0.0307 0.022 Uiso 1 1 calc R . . . .
C11 C 0.4647(5) 0.58027(17) 0.3899(6) 0.0136(11) Uani 1 1 d . . . . .
C12 C 0.5272(6) 0.59126(19) 0.5491(6) 0.0172(11) Uani 1 1 d . . . . .
H12 H 0.4894 0.6148 0.5900 0.021 Uiso 1 1 calc R . . . .
C13 C 0.6457(6) 0.56772(19) 0.6492(7) 0.0196(12) Uani 1 1 d . . . . .
H13 H 0.6887 0.5755 0.7581 0.023 Uiso 1 1 calc R . . . .
C14 C 0.7008(6) 0.5333(2) 0.5913(7) 0.0211(12) Uani 1 1 d . . . . .
H14 H 0.7825 0.5177 0.6599 0.025 Uiso 1 1 calc R . . . .
C15 C 0.6371(6) 0.52129(18) 0.4328(7) 0.0186(12) Uani 1 1 d . . . . .
H15 H 0.6740 0.4971 0.3933 0.022 Uiso 1 1 calc R . . . .
C16 C 0.5191(6) 0.54471(18) 0.3320(6) 0.0170(11) Uani 1 1 d . . . . .
H16 H 0.4754 0.5365 0.2236 0.020 Uiso 1 1 calc R . . . .
C17 C 0.6261(6) 0.6669(2) 0.1538(6) 0.0199(12) Uani 1 1 d . . . . .
C18 C 0.6400(6) 0.6243(2) 0.0663(7) 0.0244(13) Uani 1 1 d . . . . .
H18A H 0.6034 0.5978 0.1015 0.037 Uiso 1 1 calc GR . . . .
H18B H 0.7385 0.6192 0.0889 0.037 Uiso 1 1 calc GR . . . .
H18C H 0.5871 0.6285 -0.0477 0.037 Uiso 1 1 calc GR . . . .
C19 C 0.6761(6) 0.7088(2) 0.0923(8) 0.0280(14) Uani 1 1 d . . . . .
H19A H 0.6212 0.7118 -0.0218 0.042 Uiso 1 1 calc GR . . . .
H19B H 0.7748 0.7052 0.1136 0.042 Uiso 1 1 calc GR . . . .
H19C H 0.6641 0.7362 0.1459 0.042 Uiso 1 1 calc GR . . . .
C20 C 0.7190(6) 0.6599(3) 0.3312(8) 0.0362(17) Uani 1 1 d . . . . .
H20A H 0.7158 0.6873 0.3900 0.054 Uiso 1 1 calc GR . . . .
H20B H 0.8153 0.6542 0.3454 0.054 Uiso 1 1 calc GR . . . .
H20C H 0.6850 0.6337 0.3706 0.054 Uiso 1 1 calc GR . . . .
C21 C 0.0121(6) 0.67143(18) -0.1728(6) 0.0164(11) Uani 1 1 d . . . . .
C22 C -0.1015(6) 0.6695(2) -0.1100(8) 0.0274(14) Uani 1 1 d . . . . .
H22A H -0.0754 0.6473 -0.0238 0.041 Uiso 1 1 calc GR . . . .
H22B H -0.1900 0.6604 -0.1954 0.041 Uiso 1 1 calc GR . . . .
H22C H -0.1119 0.6997 -0.0706 0.041 Uiso 1 1 calc GR . . . .
C23 C 0.0024(5) 0.62830(18) -0.2696(6) 0.0169(11) Uani 1 1 d . . . . .
H23A H 0.0753 0.6289 -0.3096 0.025 Uiso 1 1 calc GR . . . .
H23B H -0.0893 0.6270 -0.3587 0.025 Uiso 1 1 calc GR . . . .
H23C H 0.0148 0.6014 -0.2025 0.025 Uiso 1 1 calc GR . . . .
C24 C -0.0091(6) 0.7132(2) -0.2786(7) 0.0231(13) Uani 1 1 d . . . . .
H24A H 0.0025 0.7410 -0.2157 0.035 Uiso 1 1 calc GR . . . .
H24B H -0.1031 0.7125 -0.3635 0.035 Uiso 1 1 calc GR . . . .
H24C H 0.0598 0.7128 -0.3246 0.035 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
Hf Cl1 2.4696(15) . ?
Hf Cl2 2.4374(15) . ?
Hf P 2.7250(17) . ?
Hf N1 1.996(4) . ?
Hf N2 2.001(4) . ?
P C2 1.855(5) . ?
P C5 1.833(5) . ?
P C11 1.828(5) . ?
N1 C3 1.480(7) . ?
N1 C17 1.476(7) . ?
N2 C4 1.473(7) . ?
N2 C21 1.488(7) . ?
C1 H1 1.0000 . ?
C1 C2 1.531(7) . ?
C1 C3 1.520(8) . ?
C1 C4 1.541(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.395(7) . ?
C5 C10 1.393(8) . ?
C6 H6 0.9500 . ?
C6 C7 1.389(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.384(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.383(8) . ?
C9 H9 0.9500 . ?
C9 C10 1.380(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(8) . ?
C11 C16 1.398(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.393(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.378(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.388(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.390(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.529(8) . ?
C17 C19 1.536(8) . ?
C17 C20 1.545(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.530(7) . ?
C21 C23 1.530(7) . ?
C21 C24 1.527(8) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
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
Cl1 Hf P 175.80(4) . . ?
Cl2 Hf Cl1 92.76(5) . . ?
Cl2 Hf P 90.97(5) . . ?
N1 Hf Cl1 97.79(13) . . ?
N1 Hf Cl2 128.91(14) . . ?
N1 Hf P 78.34(13) . . ?
N1 Hf N2 101.98(18) . . ?
N2 Hf Cl1 98.21(12) . . ?
N2 Hf Cl2 125.76(13) . . ?
N2 Hf P 81.13(12) . . ?
C2 P Hf 97.88(17) . . ?
C5 P Hf 123.97(17) . . ?
C5 P C2 103.9(2) . . ?
C11 P Hf 118.22(17) . . ?
C11 P C2 106.2(2) . . ?
C11 P C5 104.2(2) . . ?
C3 N1 Hf 117.8(4) . . ?
C17 N1 Hf 125.9(3) . . ?
C17 N1 C3 115.4(4) . . ?
C4 N2 Hf 119.0(3) . . ?
C4 N2 C21 114.2(4) . . ?
C21 N2 Hf 126.1(3) . . ?
C2 C1 H1 104.8 . . ?
C2 C1 C4 113.3(5) . . ?
C3 C1 H1 104.8 . . ?
C3 C1 C2 113.2(5) . . ?
C3 C1 C4 114.6(5) . . ?
C4 C1 H1 104.8 . . ?
P C2 H2A 108.3 . . ?
P C2 H2B 108.3 . . ?
C1 C2 P 115.8(4) . . ?
C1 C2 H2A 108.3 . . ?
C1 C2 H2B 108.3 . . ?
H2A C2 H2B 107.4 . . ?
N1 C3 C1 114.4(4) . . ?
N1 C3 H3A 108.7 . . ?
N1 C3 H3B 108.7 . . ?
C1 C3 H3A 108.7 . . ?
C1 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
N2 C4 C1 115.6(4) . . ?
N2 C4 H4A 108.4 . . ?
N2 C4 H4B 108.4 . . ?
C1 C4 H4A 108.4 . . ?
C1 C4 H4B 108.4 . . ?
H4A C4 H4B 107.4 . . ?
C6 C5 P 121.1(4) . . ?
C10 C5 P 119.1(4) . . ?
C10 C5 C6 119.7(5) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 C5 119.5(5) . . ?
C7 C6 H6 120.3 . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.7(5) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 120.3 . . ?
C9 C8 C7 119.4(5) . . ?
C9 C8 H8 120.3 . . ?
C8 C9 H9 119.6 . . ?
C10 C9 C8 120.8(5) . . ?
C10 C9 H9 119.6 . . ?
C5 C10 H10 120.1 . . ?
C9 C10 C5 119.9(5) . . ?
C9 C10 H10 120.1 . . ?
C12 C11 P 124.0(4) . . ?
C12 C11 C16 119.5(5) . . ?
C16 C11 P 116.5(4) . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 119.9(5) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.5(5) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 120.0 . . ?
C13 C14 C15 120.1(5) . . ?
C15 C14 H14 120.0 . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.8(5) . . ?
C16 C15 H15 120.1 . . ?
C11 C16 H16 119.9 . . ?
C15 C16 C11 120.2(5) . . ?
C15 C16 H16 119.9 . . ?
N1 C17 C18 107.9(4) . . ?
N1 C17 C19 110.5(5) . . ?
N1 C17 C20 111.5(5) . . ?
C18 C17 C19 109.6(5) . . ?
C18 C17 C20 107.5(5) . . ?
C19 C17 C20 109.8(5) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 C22 112.3(4) . . ?
N2 C21 C23 107.6(4) . . ?
N2 C21 C24 109.0(4) . . ?
C23 C21 C22 108.6(5) . . ?
C24 C21 C22 110.1(5) . . ?
C24 C21 C23 109.1(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 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
Hf P C2 C1 1.6(4) . . . . ?
Hf P C5 C6 -161.1(4) . . . . ?
Hf P C5 C10 19.5(5) . . . . ?
Hf P C11 C12 132.3(4) . . . . ?
Hf P C11 C16 -47.5(4) . . . . ?
Hf N1 C3 C1 32.3(6) . . . . ?
Hf N1 C17 C18 -10.5(6) . . . . ?
Hf N1 C17 C19 109.2(5) . . . . ?
Hf N1 C17 C20 -128.4(5) . . . . ?
Hf N2 C4 C1 -21.7(6) . . . . ?
Hf N2 C21 C22 135.2(4) . . . . ?
Hf N2 C21 C23 15.8(6) . . . . ?
Hf N2 C21 C24 -102.5(5) . . . . ?
P C5 C6 C7 179.9(4) . . . . ?
P C5 C10 C9 -179.9(4) . . . . ?
P C11 C12 C13 -178.1(4) . . . . ?
P C11 C16 C15 178.3(4) . . . . ?
C2 P C5 C6 -51.5(5) . . . . ?
C2 P C5 C10 129.2(4) . . . . ?
C2 P C11 C12 23.8(5) . . . . ?
C2 P C11 C16 -156.0(4) . . . . ?
C2 C1 C3 N1 60.2(6) . . . . ?
C2 C1 C4 N2 -66.5(6) . . . . ?
C3 N1 C17 C18 -179.4(5) . . . . ?
C3 N1 C17 C19 -59.6(6) . . . . ?
C3 N1 C17 C20 62.8(7) . . . . ?
C3 C1 C2 P -67.4(5) . . . . ?
C3 C1 C4 N2 65.6(6) . . . . ?
C4 N2 C21 C22 -54.9(6) . . . . ?
C4 N2 C21 C23 -174.4(4) . . . . ?
C4 N2 C21 C24 67.4(6) . . . . ?
C4 C1 C2 P 65.3(6) . . . . ?
C4 C1 C3 N1 -71.9(6) . . . . ?
C5 P C2 C1 -126.4(4) . . . . ?
C5 P C11 C12 -85.5(5) . . . . ?
C5 P C11 C16 94.6(4) . . . . ?
C5 C6 C7 C8 0.6(8) . . . . ?
C6 C5 C10 C9 0.7(8) . . . . ?
C6 C7 C8 C9 -0.4(9) . . . . ?
C7 C8 C9 C10 0.3(9) . . . . ?
C8 C9 C10 C5 -0.5(8) . . . . ?
C10 C5 C6 C7 -0.8(8) . . . . ?
C11 P C2 C1 124.1(4) . . . . ?
C11 P C5 C6 59.5(5) . . . . ?
C11 P C5 C10 -119.8(4) . . . . ?
C11 C12 C13 C14 -0.5(8) . . . . ?
C12 C11 C16 C15 -1.5(8) . . . . ?
C12 C13 C14 C15 -1.1(8) . . . . ?
C13 C14 C15 C16 1.3(8) . . . . ?
C14 C15 C16 C11 0.0(8) . . . . ?
C16 C11 C12 C13 1.7(8) . . . . ?
C17 N1 C3 C1 -157.9(5) . . . . ?
C21 N2 C4 C1 167.7(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_detector                 'CCD plate'
####################################################################### 
# 
# 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_ba_tk1
_database_code_depnum_ccdc_archive 'CCDC 1440958'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;
_audit_creation_date             
;
'Mon Jan 19 15:06:46 2015'
;

_audit_block_code                ba_tk1
_audit_block_refno               2296
_audit_block_usercomment         'TK50, needle, colourless'


_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C38 H49 N2 P Zr'
_chemical_formula_sum            'C38 H49 N2 P Zr'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         655.98
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      120(1)
_chemical_oxdiff_formula         'C38 H47 N2 P Zr'
_chemical_oxdiff_usercomment     'TK50, needle, colourless'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 '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'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_h-m   'P b c a'
_symmetry_int_tables_number      61
_chemical_absolute_configuration .

_space_group_name_Hall           '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.53716(5)
_cell_length_b                   19.78721(7)
_cell_length_c                   20.54069(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6721.41(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    104222
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.6880
_cell_measurement_theta_min      4.0810
_shelx_estimated_absorpt_T_max   0.923
_shelx_estimated_absorpt_T_min   0.590
_exptl_absorpt_coefficient_mu    3.330
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.024
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            242838
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.863
_diffrn_reflns_theta_min         4.095
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -68.00   15.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   60.0000 83

#__ type_ start__ end____ width___ exp.time_
  2 omega   12.00   68.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  120.0000 56

#__ type_ start__ end____ width___ exp.time_
  3 omega  -21.00    7.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  120.0000 28

#__ type_ start__ end____ width___ exp.time_
  4 omega  -29.00   37.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000    0.0000 66

#__ type_ start__ end____ width___ exp.time_
  5 omega  -69.00   10.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -30.0000 79

#__ type_ start__ end____ width___ exp.time_
  6 omega  -61.00   24.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000 -180.0000 85

#__ type_ start__ end____ width___ exp.time_
  7 omega    2.00   83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000   90.0000 81

#__ type_ start__ end____ width___ exp.time_
  8 omega   24.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 92

#__ type_ start__ end____ width___ exp.time_
  9 omega   24.00   56.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 32

#__ type_ start__ end____ width___ exp.time_
 10 omega  -12.00   74.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -60.0000 86

#__ type_ start__ end____ width___ exp.time_
 11 omega   55.00  121.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 66

#__ type_ start__ end____ width___ exp.time_
 12 omega   75.00  122.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 47

#__ type_ start__ end____ width___ exp.time_
 13 omega    9.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   90.0000 60

#__ type_ start__ end____ width___ exp.time_
 14 omega   24.00   50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 15 omega   24.00  123.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 99

#__ type_ start__ end____ width___ exp.time_
 16 omega   24.00  121.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -180.0000 97

#__ type_ start__ end____ width___ exp.time_
 17 omega   23.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -74.6559 25

#__ type_ start__ end____ width___ exp.time_
 18 omega   24.00   62.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 38

#__ type_ start__ end____ width___ exp.time_
 19 omega  -16.00   84.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -150.0000 100

#__ type_ start__ end____ width___ exp.time_
 20 omega   24.00   50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 21 omega   59.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 50

#__ type_ start__ end____ width___ exp.time_
 22 omega   25.00   54.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 29

#__ type_ start__ end____ width___ exp.time_
 23 omega   79.00  120.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 41

#__ type_ start__ end____ width___ exp.time_
 24 omega   24.00   52.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 28

#__ type_ start__ end____ width___ exp.time_
 25 omega   24.00   50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 26 omega   24.00   58.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 34

#__ type_ start__ end____ width___ exp.time_
 27 omega   73.00  123.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 50

#__ type_ start__ end____ width___ exp.time_
 28 omega   82.00  115.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -90.0000 33

#__ type_ start__ end____ width___ exp.time_
 29 omega  118.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 60

#__ type_ start__ end____ width___ exp.time_
 30 omega   44.00  102.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -180.0000 58

#__ type_ start__ end____ width___ exp.time_
 31 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 32 omega   39.00  103.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000 -120.0000 64

#__ type_ start__ end____ width___ exp.time_
 33 omega   81.00  106.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   71.0000   22.9812 25

#__ type_ start__ end____ width___ exp.time_
 34 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -114.9018 26

#__ type_ start__ end____ width___ exp.time_
 35 omega   38.00  103.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000   30.0000 65

#__ type_ start__ end____ width___ exp.time_
 36 omega   82.00  174.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -120.0000 92

#__ type_ start__ end____ width___ exp.time_
 37 omega  110.00  152.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000   65.5822 42

#__ type_ start__ end____ width___ exp.time_
 38 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
 39 omega   49.00  114.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 65

#__ type_ start__ end____ width___ exp.time_
 40 omega   79.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000   65.5822 30

#__ type_ start__ end____ width___ exp.time_
 41 omega   79.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000   55.5534 26

#__ type_ start__ end____ width___ exp.time_
 42 omega   83.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   40.0000 -160.4271 94

#__ type_ start__ end____ width___ exp.time_
 43 omega  109.00  162.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 53

#__ type_ start__ end____ width___ exp.time_
 44 omega   78.00  103.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
 45 omega  118.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 60

#__ type_ start__ end____ width___ exp.time_
 46 omega   78.00  103.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 25

#__ type_ start__ end____ width___ exp.time_
 47 omega   81.00  106.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   72.0000  172.0864 25

#__ type_ start__ end____ width___ exp.time_
 48 omega   80.00  166.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000 -102.8439 86

#__ type_ start__ end____ width___ exp.time_
 49 omega   83.00  120.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   35.0000  148.3004 37

#__ type_ start__ end____ width___ exp.time_
 50 omega  109.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 68

#__ type_ start__ end____ width___ exp.time_
 51 omega   78.00  116.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 38

#__ type_ start__ end____ width___ exp.time_
 52 omega   78.00  175.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 97

#__ type_ start__ end____ width___ exp.time_
 53 omega   41.00  146.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000 -120.0000 105

#__ type_ start__ end____ width___ exp.time_
 54 omega   78.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 99

#__ type_ start__ end____ width___ exp.time_
 55 omega   78.00  103.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 56 omega   85.00  170.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 85

#__ type_ start__ end____ width___ exp.time_
 57 omega   85.00  111.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
 58 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
 59 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   47.3454 26

#__ type_ start__ end____ width___ exp.time_
 60 omega   85.00  110.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
 61 omega   85.00  111.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
 62 omega   82.00  150.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  120.0000 68

#__ type_ start__ end____ width___ exp.time_
 63 omega   78.00  103.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 25

#__ type_ start__ end____ width___ exp.time_
 64 omega  141.00  167.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 65 omega   78.00  103.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
 66 omega   56.00  115.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 59

#__ type_ start__ end____ width___ exp.time_
 67 omega   67.00   97.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  120.0000 30

#__ type_ start__ end____ width___ exp.time_
 68 omega   78.00  162.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -74.9057 84

#__ type_ start__ end____ width___ exp.time_
 69 omega   79.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000  -19.8129 29

#__ type_ start__ end____ width___ exp.time_
 70 omega   84.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   41.0000  168.1117 25

#__ type_ start__ end____ width___ exp.time_
 71 omega  -26.00   72.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -60.0000 98

#__ type_ start__ end____ width___ exp.time_
 72 omega  -21.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   60.0000 90

#__ type_ start__ end____ width___ exp.time_
 73 omega  -26.00   72.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000   30.0000 98

#__ type_ start__ end____ width___ exp.time_
 74 omega  -26.00   72.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000 -120.0000 98

#__ type_ start__ end____ width___ exp.time_
 75 omega  -73.00   73.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000 -180.0000 146

#__ type_ start__ end____ width___ exp.time_
 76 omega  -69.00   21.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -120.0000 90

#__ type_ start__ end____ width___ exp.time_
 77 omega  -15.00   75.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000 -180.0000 90

#__ type_ start__ end____ width___ exp.time_
 78 omega   24.00  124.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 100

#__ type_ start__ end____ width___ exp.time_
 79 omega    1.00   96.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000  150.0000 95

#__ type_ start__ end____ width___ exp.time_
 80 omega   23.00  111.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000  -30.0000 88

#__ type_ start__ end____ width___ exp.time_
 81 omega  -15.00   75.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000    0.0000 90

#__ type_ start__ end____ width___ exp.time_
 82 omega   23.00   49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -74.6559 26

#__ type_ start__ end____ width___ exp.time_
 83 omega   24.00  124.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 100

#__ type_ start__ end____ width___ exp.time_
 84 omega   24.00  124.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 100

#__ type_ start__ end____ width___ exp.time_
 85 omega   33.00  123.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -150.0000 90

#__ type_ start__ end____ width___ exp.time_
 86 omega   33.00  123.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000   90.0000 90

#__ type_ start__ end____ width___ exp.time_
 87 omega   24.00  124.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 100

#__ type_ start__ end____ width___ exp.time_
 88 omega   24.00  124.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 100

#__ type_ start__ end____ width___ exp.time_
 89 omega  -18.00   80.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000 -150.0000 98

#__ type_ start__ end____ width___ exp.time_
 90 omega   24.00  124.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 100

#__ type_ start__ end____ width___ exp.time_
 91 omega  -19.00   86.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -28.0000  -85.0000 105

#__ type_ start__ end____ width___ exp.time_
 92 omega   24.00  124.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 100

#__ type_ start__ end____ width___ exp.time_
 93 omega   33.00  123.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000   60.0000 90

#__ type_ start__ end____ width___ exp.time_
 94 omega  -19.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -19.0000   30.0000 117

#__ type_ start__ end____ width___ exp.time_
 95 omega   85.00  175.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 90

#__ type_ start__ end____ width___ exp.time_
 96 omega   82.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -30.0000 96

#__ type_ start__ end____ width___ exp.time_
 97 omega   36.00  116.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -60.0000 80

#__ type_ start__ end____ width___ exp.time_
 98 omega   35.00   94.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   30.0000 59

#__ type_ start__ end____ width___ exp.time_
 99 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 100

#__ type_ start__ end____ width___ exp.time_
100 omega   86.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000   30.0000 92

#__ type_ start__ end____ width___ exp.time_
101 omega  100.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  150.0000 78

#__ type_ start__ end____ width___ exp.time_
102 omega   85.00  175.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 90

#__ type_ start__ end____ width___ exp.time_
103 omega   35.00   94.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  150.0000 59

#__ type_ start__ end____ width___ exp.time_
104 omega   85.00  175.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 90

#__ type_ start__ end____ width___ exp.time_
105 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 100

#__ type_ start__ end____ width___ exp.time_
106 omega   85.00  175.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 90

#__ type_ start__ end____ width___ exp.time_
107 omega   86.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  -30.0000 92

#__ type_ start__ end____ width___ exp.time_
108 omega   85.00  175.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 90

#__ type_ start__ end____ width___ exp.time_
109 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 100

#__ type_ start__ end____ width___ exp.time_
110 omega   38.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  150.0000 66

#__ type_ start__ end____ width___ exp.time_
111 omega   80.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000  118.2945 98

#__ type_ start__ end____ width___ exp.time_
112 omega   86.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000 -120.0000 92

#__ type_ start__ end____ width___ exp.time_
113 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -74.9057 100

#__ type_ start__ end____ width___ exp.time_
114 omega   82.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000    0.0000 96

#__ type_ start__ end____ width___ exp.time_
115 omega   86.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000   60.0000 92

#__ type_ start__ end____ width___ exp.time_
116 omega   80.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   73.0000   26.0404 97

#__ type_ start__ end____ width___ exp.time_
117 omega   36.00  116.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 80

#__ type_ start__ end____ width___ exp.time_
118 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 100

#__ type_ start__ end____ width___ exp.time_
119 omega   86.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  -80.0557 92

#__ type_ start__ end____ width___ exp.time_
120 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 100

#__ type_ start__ end____ width___ exp.time_
121 omega   36.00  146.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000   90.0000 110

#__ type_ start__ end____ width___ exp.time_
122 omega   36.00  116.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 80

#__ type_ start__ end____ width___ exp.time_
123 omega   80.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000 -102.8439 98

#__ type_ start__ end____ width___ exp.time_
124 omega   86.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000 -150.0000 92

#__ type_ start__ end____ width___ exp.time_
125 omega  -21.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   90.0000 90

#__ type_ start__ end____ width___ exp.time_
126 omega  -21.00   53.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -30.0000 74

#__ type_ start__ end____ width___ exp.time_
127 omega  -21.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 90

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0242430000
_diffrn_orient_matrix_UB_12      -0.0695941000
_diffrn_orient_matrix_UB_13      0.0273708000
_diffrn_orient_matrix_UB_21      -0.0896554000
_diffrn_orient_matrix_UB_22      0.0210155000
_diffrn_orient_matrix_UB_23      -0.0019052000
_diffrn_orient_matrix_UB_31      -0.0070263000
_diffrn_orient_matrix_UB_32      -0.0279224000
_diffrn_orient_matrix_UB_33      -0.0697963000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6236
_reflns_number_total             6477
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6477
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0228
_refine_ls_restrained_S_all      1.076
_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)+(0.0250P)²+4.6715P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0562
_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 Ternary CH refined with riding coordinates:
 C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C25(H25A,H25B), C32(H32A,H32B)
2.c 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), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C34(H34),
  C35(H35), C36(H36), C37(H37), C38(H38)
2.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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 0.55067(2) 0.44672(2) 0.18490(2) 0.01301(5) Uani 1 1 d . . . . .
P P 0.54013(2) 0.43511(2) 0.32280(2) 0.01706(8) Uani 1 1 d . . . . .
N1 N 0.63885(7) 0.37774(6) 0.20112(6) 0.0177(3) Uani 1 1 d . . . . .
N2 N 0.60004(7) 0.53562(6) 0.21710(6) 0.0170(2) Uani 1 1 d . . . . .
C1 C 0.64870(10) 0.45246(10) 0.33769(8) 0.0280(4) Uani 1 1 d . . . . .
H1A H 0.6527 0.4933 0.3653 0.034 Uiso 1 1 calc R . . . .
H1B H 0.6712 0.4143 0.3630 0.034 Uiso 1 1 calc R . . . .
C2 C 0.70250(8) 0.46319(8) 0.27761(8) 0.0181(3) Uani 1 1 d . . . . .
H2 H 0.7577 0.4708 0.2962 0.022 Uiso 1 1 calc R . . . .
C3 C 0.71282(9) 0.40091(8) 0.23393(9) 0.0247(3) Uani 1 1 d . . . . .
H3A H 0.7539 0.4113 0.2004 0.030 Uiso 1 1 calc R . . . .
H3B H 0.7341 0.3634 0.2608 0.030 Uiso 1 1 calc R . . . .
C4 C 0.68341(9) 0.52912(8) 0.24202(8) 0.0229(3) Uani 1 1 d . . . . .
H4A H 0.6940 0.5672 0.2721 0.027 Uiso 1 1 calc R . . . .
H4B H 0.7212 0.5337 0.2049 0.027 Uiso 1 1 calc R . . . .
C5 C 0.51611(9) 0.36327(8) 0.37610(7) 0.0179(3) Uani 1 1 d . . . . .
C6 C 0.57380(10) 0.31905(8) 0.40124(8) 0.0244(3) Uani 1 1 d . . . . .
H6 H 0.6290 0.3242 0.3894 0.029 Uiso 1 1 calc R . . . .
C7 C 0.55129(10) 0.26746(8) 0.44342(9) 0.0286(4) Uani 1 1 d . . . . .
H7 H 0.5914 0.2381 0.4605 0.034 Uiso 1 1 calc R . . . .
C8 C 0.47132(10) 0.25831(8) 0.46076(9) 0.0262(3) Uani 1 1 d . . . . .
H8 H 0.4565 0.2233 0.4901 0.031 Uiso 1 1 calc R . . . .
C9 C 0.41294(10) 0.30098(8) 0.43477(8) 0.0237(3) Uani 1 1 d . . . . .
H9 H 0.3577 0.2948 0.4460 0.028 Uiso 1 1 calc R . . . .
C10 C 0.43482(9) 0.35253(8) 0.39259(8) 0.0206(3) Uani 1 1 d . . . . .
H10 H 0.3942 0.3809 0.3746 0.025 Uiso 1 1 calc R . . . .
C11 C 0.48656(9) 0.50308(8) 0.36535(7) 0.0184(3) Uani 1 1 d . . . . .
C12 C 0.51593(10) 0.53264(8) 0.42226(8) 0.0235(3) Uani 1 1 d . . . . .
H12 H 0.5647 0.5164 0.4410 0.028 Uiso 1 1 calc R . . . .
C13 C 0.47462(11) 0.58548(8) 0.45178(8) 0.0270(4) Uani 1 1 d . . . . .
H13 H 0.4959 0.6057 0.4901 0.032 Uiso 1 1 calc R . . . .
C14 C 0.40269(10) 0.60881(8) 0.42572(8) 0.0255(3) Uani 1 1 d . . . . .
H14 H 0.3745 0.6449 0.4461 0.031 Uiso 1 1 calc R . . . .
C15 C 0.37202(10) 0.57933(8) 0.36978(8) 0.0235(3) Uani 1 1 d . . . . .
H15 H 0.3226 0.5951 0.3519 0.028 Uiso 1 1 calc R . . . .
C16 C 0.41335(9) 0.52668(8) 0.33973(8) 0.0206(3) Uani 1 1 d . . . . .
H16 H 0.3917 0.5066 0.3015 0.025 Uiso 1 1 calc R . . . .
C17 C 0.63897(9) 0.30656(8) 0.17928(7) 0.0193(3) Uani 1 1 d . . . . .
C18 C 0.64030(11) 0.25768(8) 0.23720(9) 0.0287(4) Uani 1 1 d . . . . .
H18A H 0.6907 0.2637 0.2617 0.043 Uiso 1 1 calc GR . . . .
H18B H 0.6370 0.2111 0.2213 0.043 Uiso 1 1 calc GR . . . .
H18C H 0.5941 0.2670 0.2657 0.043 Uiso 1 1 calc GR . . . .
C19 C 0.56044(10) 0.29656(8) 0.14145(9) 0.0259(3) Uani 1 1 d . . . . .
H19A H 0.5143 0.3071 0.1697 0.039 Uiso 1 1 calc GR . . . .
H19B H 0.5567 0.2495 0.1269 0.039 Uiso 1 1 calc GR . . . .
H19C H 0.5599 0.3266 0.1036 0.039 Uiso 1 1 calc GR . . . .
C20 C 0.71107(10) 0.29259(8) 0.13433(9) 0.0261(3) Uani 1 1 d . . . . .
H20A H 0.7107 0.3250 0.0982 0.039 Uiso 1 1 calc GR . . . .
H20B H 0.7071 0.2466 0.1170 0.039 Uiso 1 1 calc GR . . . .
H20C H 0.7615 0.2973 0.1590 0.039 Uiso 1 1 calc GR . . . .
C21 C 0.57288(9) 0.60684(8) 0.20910(8) 0.0211(3) Uani 1 1 d . . . . .
C22 C 0.57329(11) 0.64624(8) 0.27355(9) 0.0299(4) Uani 1 1 d . . . . .
H22A H 0.5415 0.6216 0.3061 0.045 Uiso 1 1 calc GR . . . .
H22B H 0.5496 0.6911 0.2667 0.045 Uiso 1 1 calc GR . . . .
H22C H 0.6291 0.6511 0.2890 0.045 Uiso 1 1 calc GR . . . .
C23 C 0.48563(10) 0.60545(8) 0.18399(8) 0.0242(3) Uani 1 1 d . . . . .
H23A H 0.4831 0.5790 0.1437 0.036 Uiso 1 1 calc GR . . . .
H23B H 0.4674 0.6517 0.1754 0.036 Uiso 1 1 calc GR . . . .
H23C H 0.4505 0.5847 0.2168 0.036 Uiso 1 1 calc GR . . . .
C24 C 0.62655(11) 0.64336(9) 0.15953(10) 0.0330(4) Uani 1 1 d . . . . .
H24A H 0.6822 0.6452 0.1759 0.049 Uiso 1 1 calc GR . . . .
H24B H 0.6064 0.6894 0.1529 0.049 Uiso 1 1 calc GR . . . .
H24C H 0.6254 0.6189 0.1181 0.049 Uiso 1 1 calc GR . . . .
C25 C 0.41160(9) 0.42717(8) 0.18085(8) 0.0203(3) Uani 1 1 d . . . . .
H25A H 0.3968 0.4099 0.2245 0.024 Uiso 1 1 calc R . . . .
H25B H 0.3864 0.4724 0.1771 0.024 Uiso 1 1 calc R . . . .
C26 C 0.36786(8) 0.38372(7) 0.13393(7) 0.0166(3) Uani 1 1 d . . . . .
C27 C 0.35072(9) 0.31594(8) 0.14834(8) 0.0213(3) Uani 1 1 d . . . . .
H27 H 0.3673 0.2979 0.1890 0.026 Uiso 1 1 calc R . . . .
C28 C 0.31018(10) 0.27465(8) 0.10466(9) 0.0265(4) Uani 1 1 d . . . . .
H28 H 0.3001 0.2288 0.1156 0.032 Uiso 1 1 calc R . . . .
C29 C 0.28423(9) 0.29974(9) 0.04530(9) 0.0278(4) Uani 1 1 d . . . . .
H29 H 0.2562 0.2715 0.0155 0.033 Uiso 1 1 calc R . . . .
C30 C 0.29993(9) 0.36678(9) 0.03019(8) 0.0270(4) Uani 1 1 d . . . . .
H30 H 0.2823 0.3847 -0.0103 0.032 Uiso 1 1 calc R . . . .
C31 C 0.34112(9) 0.40803(8) 0.07360(8) 0.0219(3) Uani 1 1 d . . . . .
H31 H 0.3514 0.4538 0.0622 0.026 Uiso 1 1 calc R . . . .
C32 C 0.55505(9) 0.46817(9) 0.07346(8) 0.0225(3) Uani 1 1 d . . . . .
H32A H 0.5077 0.4458 0.0533 0.027 Uiso 1 1 calc R . . . .
H32B H 0.5482 0.5174 0.0671 0.027 Uiso 1 1 calc R . . . .
C33 C 0.62814(9) 0.44689(7) 0.03707(7) 0.0190(3) Uani 1 1 d . . . . .
C34 C 0.62358(10) 0.40192(8) -0.01538(8) 0.0216(3) Uani 1 1 d . . . . .
H34 H 0.5724 0.3845 -0.0279 0.026 Uiso 1 1 calc R . . . .
C35 C 0.69227(10) 0.38206(8) -0.04962(8) 0.0263(3) Uani 1 1 d . . . . .
H35 H 0.6872 0.3516 -0.0851 0.032 Uiso 1 1 calc R . . . .
C36 C 0.76800(10) 0.40630(8) -0.03239(9) 0.0273(4) Uani 1 1 d . . . . .
H36 H 0.8149 0.3926 -0.0556 0.033 Uiso 1 1 calc R . . . .
C37 C 0.77393(10) 0.45103(8) 0.01955(8) 0.0255(3) Uani 1 1 d . . . . .
H37 H 0.8253 0.4682 0.0319 0.031 Uiso 1 1 calc R . . . .
C38 C 0.70571(10) 0.47072(8) 0.05346(8) 0.0215(3) Uani 1 1 d . . . . .
H38 H 0.7113 0.5013 0.0889 0.026 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
Zr P 2.8472(4) . ?
Zr N1 2.0250(12) . ?
Zr N2 2.0489(12) . ?
Zr C25 2.3336(15) . ?
Zr C32 2.3292(16) . ?
P C1 1.8534(16) . ?
P C5 1.8377(16) . ?
P C11 1.8323(16) . ?
N1 C3 1.4699(19) . ?
N1 C17 1.4782(19) . ?
N2 C4 1.4763(19) . ?
N2 C21 1.4882(18) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.536(2) . ?
C2 H2 1.0000 . ?
C2 C3 1.534(2) . ?
C2 C4 1.528(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.394(2) . ?
C5 C10 1.402(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.390(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.381(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.389(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.386(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.395(2) . ?
C11 C16 1.400(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.388(2) . ?
C13 H13 0.9500 . ?
C13 C14 1.384(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.385(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.391(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.534(2) . ?
C17 C19 1.526(2) . ?
C17 C20 1.533(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.536(2) . ?
C21 C23 1.533(2) . ?
C21 C24 1.532(2) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.480(2) . ?
C26 C27 1.402(2) . ?
C26 C31 1.401(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.386(2) . ?
C28 H28 0.9500 . ?
C28 C29 1.385(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.387(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.388(2) . ?
C31 H31 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.482(2) . ?
C33 C34 1.399(2) . ?
C33 C38 1.408(2) . ?
C34 H34 0.9500 . ?
C34 C35 1.393(2) . ?
C35 H35 0.9500 . ?
C35 C36 1.387(2) . ?
C36 H36 0.9500 . ?
C36 C37 1.390(2) . ?
C37 H37 0.9500 . ?
C37 C38 1.382(2) . ?
C38 H38 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 Zr P 79.98(4) . . ?
N1 Zr N2 103.80(5) . . ?
N1 Zr C25 127.15(5) . . ?
N1 Zr C32 105.20(5) . . ?
N2 Zr P 76.85(4) . . ?
N2 Zr C25 123.13(5) . . ?
N2 Zr C32 98.53(6) . . ?
C25 Zr P 87.81(4) . . ?
C32 Zr P 173.89(4) . . ?
C32 Zr C25 91.48(5) . . ?
C1 P Zr 95.16(5) . . ?
C5 P Zr 131.94(5) . . ?
C5 P C1 104.74(7) . . ?
C11 P Zr 116.42(5) . . ?
C11 P C1 104.70(8) . . ?
C11 P C5 100.31(7) . . ?
C3 N1 Zr 117.68(9) . . ?
C3 N1 C17 115.80(12) . . ?
C17 N1 Zr 126.39(10) . . ?
C4 N2 Zr 114.16(9) . . ?
C4 N2 C21 113.74(12) . . ?
C21 N2 Zr 131.08(9) . . ?
P C1 H1A 108.0 . . ?
P C1 H1B 108.0 . . ?
H1A C1 H1B 107.3 . . ?
C2 C1 P 117.00(11) . . ?
C2 C1 H1A 108.0 . . ?
C2 C1 H1B 108.0 . . ?
C1 C2 H2 104.0 . . ?
C3 C2 C1 115.04(14) . . ?
C3 C2 H2 104.0 . . ?
C4 C2 C1 112.49(13) . . ?
C4 C2 H2 104.0 . . ?
C4 C2 C3 115.41(14) . . ?
N1 C3 C2 115.23(12) . . ?
N1 C3 H3A 108.5 . . ?
N1 C3 H3B 108.5 . . ?
C2 C3 H3A 108.5 . . ?
C2 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
N2 C4 C2 115.66(12) . . ?
N2 C4 H4A 108.4 . . ?
N2 C4 H4B 108.4 . . ?
C2 C4 H4A 108.4 . . ?
C2 C4 H4B 108.4 . . ?
H4A C4 H4B 107.4 . . ?
C6 C5 P 123.94(12) . . ?
C6 C5 C10 118.13(14) . . ?
C10 C5 P 117.92(11) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.59(15) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.89(15) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 120.4 . . ?
C7 C8 C9 119.11(16) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.40(15) . . ?
C10 C9 H9 119.8 . . ?
C5 C10 H10 119.6 . . ?
C9 C10 C5 120.83(14) . . ?
C9 C10 H10 119.6 . . ?
C12 C11 P 122.64(12) . . ?
C12 C11 C16 118.44(14) . . ?
C16 C11 P 118.92(11) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.71(15) . . ?
C13 C12 H12 119.6 . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.35(15) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 120.2 . . ?
C13 C14 C15 119.69(15) . . ?
C15 C14 H14 120.2 . . ?
C14 C15 H15 119.9 . . ?
C14 C15 C16 120.25(15) . . ?
C16 C15 H15 119.9 . . ?
C11 C16 H16 119.7 . . ?
C15 C16 C11 120.54(14) . . ?
C15 C16 H16 119.7 . . ?
N1 C17 C18 111.44(13) . . ?
N1 C17 C19 106.08(12) . . ?
N1 C17 C20 110.83(12) . . ?
C19 C17 C18 108.99(14) . . ?
C19 C17 C20 109.38(13) . . ?
C20 C17 C18 110.02(13) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 C22 112.58(13) . . ?
N2 C21 C23 107.71(12) . . ?
N2 C21 C24 110.20(13) . . ?
C23 C21 C22 107.65(13) . . ?
C24 C21 C22 109.32(14) . . ?
C24 C21 C23 109.29(14) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Zr C25 H25A 105.6 . . ?
Zr C25 H25B 105.6 . . ?
H25A C25 H25B 106.1 . . ?
C26 C25 Zr 126.95(10) . . ?
C26 C25 H25A 105.6 . . ?
C26 C25 H25B 105.6 . . ?
C27 C26 C25 121.13(14) . . ?
C31 C26 C25 122.05(14) . . ?
C31 C26 C27 116.82(14) . . ?
C26 C27 H27 119.2 . . ?
C28 C27 C26 121.65(15) . . ?
C28 C27 H27 119.2 . . ?
C27 C28 H28 119.7 . . ?
C29 C28 C27 120.57(15) . . ?
C29 C28 H28 119.7 . . ?
C28 C29 H29 120.6 . . ?
C28 C29 C30 118.81(15) . . ?
C30 C29 H29 120.6 . . ?
C29 C30 H30 119.6 . . ?
C29 C30 C31 120.71(16) . . ?
C31 C30 H30 119.6 . . ?
C26 C31 H31 119.3 . . ?
C30 C31 C26 121.43(15) . . ?
C30 C31 H31 119.3 . . ?
Zr C32 H32A 107.8 . . ?
Zr C32 H32B 107.8 . . ?
H32A C32 H32B 107.1 . . ?
C33 C32 Zr 117.98(10) . . ?
C33 C32 H32A 107.8 . . ?
C33 C32 H32B 107.8 . . ?
C34 C33 C32 121.67(14) . . ?
C34 C33 C38 116.50(14) . . ?
C38 C33 C32 121.83(14) . . ?
C33 C34 H34 119.2 . . ?
C35 C34 C33 121.63(15) . . ?
C35 C34 H34 119.2 . . ?
C34 C35 H35 119.7 . . ?
C36 C35 C34 120.66(15) . . ?
C36 C35 H35 119.7 . . ?
C35 C36 H36 120.7 . . ?
C35 C36 C37 118.68(15) . . ?
C37 C36 H36 120.7 . . ?
C36 C37 H37 119.7 . . ?
C38 C37 C36 120.59(15) . . ?
C38 C37 H37 119.7 . . ?
C33 C38 H38 119.0 . . ?
C37 C38 C33 121.94(15) . . ?
C37 C38 H38 119.0 . . ?

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
Zr P C1 C2 -2.16(14) . . . . ?
Zr P C5 C6 90.39(14) . . . . ?
Zr P C5 C10 -89.84(13) . . . . ?
Zr P C11 C12 -135.61(12) . . . . ?
Zr P C11 C16 44.09(13) . . . . ?
Zr N1 C3 C2 25.45(18) . . . . ?
Zr N1 C17 C18 -117.53(13) . . . . ?
Zr N1 C17 C19 0.96(17) . . . . ?
Zr N1 C17 C20 119.59(13) . . . . ?
Zr N2 C4 C2 -35.03(17) . . . . ?
Zr N2 C21 C22 131.72(13) . . . . ?
Zr N2 C21 C23 13.20(19) . . . . ?
Zr N2 C21 C24 -105.95(15) . . . . ?
Zr C25 C26 C27 93.31(16) . . . . ?
Zr C25 C26 C31 -87.20(17) . . . . ?
Zr C32 C33 C34 121.51(14) . . . . ?
Zr C32 C33 C38 -58.41(18) . . . . ?
P C1 C2 C3 -65.89(17) . . . . ?
P C1 C2 C4 69.03(17) . . . . ?
P C5 C6 C7 177.37(13) . . . . ?
P C5 C10 C9 -177.29(12) . . . . ?
P C11 C12 C13 177.95(13) . . . . ?
P C11 C16 C15 -178.38(12) . . . . ?
C1 P C5 C6 -20.80(15) . . . . ?
C1 P C5 C10 158.97(12) . . . . ?
C1 P C11 C12 -32.07(15) . . . . ?
C1 P C11 C16 147.64(12) . . . . ?
C1 C2 C3 N1 65.71(18) . . . . ?
C1 C2 C4 N2 -60.04(18) . . . . ?
C3 N1 C17 C18 66.81(17) . . . . ?
C3 N1 C17 C19 -174.70(13) . . . . ?
C3 N1 C17 C20 -56.07(18) . . . . ?
C3 C2 C4 N2 74.70(17) . . . . ?
C4 N2 C21 C22 -60.73(17) . . . . ?
C4 N2 C21 C23 -179.25(13) . . . . ?
C4 N2 C21 C24 61.60(18) . . . . ?
C4 C2 C3 N1 -67.87(18) . . . . ?
C5 P C1 C2 133.70(13) . . . . ?
C5 P C11 C12 76.30(14) . . . . ?
C5 P C11 C16 -104.00(12) . . . . ?
C5 C6 C7 C8 0.8(3) . . . . ?
C6 C5 C10 C9 2.5(2) . . . . ?
C6 C7 C8 C9 0.8(3) . . . . ?
C7 C8 C9 C10 -0.7(3) . . . . ?
C8 C9 C10 C5 -0.9(2) . . . . ?
C10 C5 C6 C7 -2.4(2) . . . . ?
C11 P C1 C2 -121.21(13) . . . . ?
C11 P C5 C6 -129.13(14) . . . . ?
C11 P C5 C10 50.64(13) . . . . ?
C11 C12 C13 C14 1.2(3) . . . . ?
C12 C11 C16 C15 1.3(2) . . . . ?
C12 C13 C14 C15 -0.2(3) . . . . ?
C13 C14 C15 C16 -0.2(2) . . . . ?
C14 C15 C16 C11 -0.4(2) . . . . ?
C16 C11 C12 C13 -1.8(2) . . . . ?
C17 N1 C3 C2 -158.49(13) . . . . ?
C21 N2 C4 C2 155.22(14) . . . . ?
C25 C26 C27 C28 -179.66(14) . . . . ?
C25 C26 C31 C30 -179.77(14) . . . . ?
C26 C27 C28 C29 -0.9(2) . . . . ?
C27 C26 C31 C30 -0.3(2) . . . . ?
C27 C28 C29 C30 0.3(2) . . . . ?
C28 C29 C30 C31 0.2(2) . . . . ?
C29 C30 C31 C26 -0.3(2) . . . . ?
C31 C26 C27 C28 0.8(2) . . . . ?
C32 C33 C34 C35 179.87(15) . . . . ?
C32 C33 C38 C37 -179.91(15) . . . . ?
C33 C34 C35 C36 0.3(3) . . . . ?
C34 C33 C38 C37 0.2(2) . . . . ?
C34 C35 C36 C37 -0.3(3) . . . . ?
C35 C36 C37 C38 0.2(3) . . . . ?
C36 C37 C38 C33 -0.2(2) . . . . ?
C38 C33 C34 C35 -0.2(2) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -5 -12 0.0312 0.0003 -5.0004 -12.0002 0.0195 -0.0823 0.9772
-10 3 -1 0.0821 -9.9999 3.0009 -1.0002 0.0062 0.9615 0.0563
9 -5 -4 0.0713 9.0000 -5.0010 -3.9999 0.0204 -0.9044 0.3556
3 4 12 0.0442 2.9997 4.0001 12.0002 -0.0227 -0.2077 -0.9703
3 12 -5 0.0122 3.0003 12.0000 -5.0000 -1.0447 -0.0073 -0.0072
-3 -12 5 0.0122 -3.0003 -12.0000 5.0000 1.0447 0.0073 0.0072

_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            16.54016(16)
_cell_oxdiff_length_b            19.7823(2)
_cell_oxdiff_length_c            20.5421(3)
_cell_oxdiff_angle_alpha         90.0392(10)
_cell_oxdiff_angle_beta          89.9809(9)
_cell_oxdiff_angle_gamma         89.9938(9)
_cell_oxdiff_volume              6721.41(14)
_cell_oxdiff_measurement_reflns_used 104222
_diffrn_measurement_specimen_support 'polyimid foil'



