# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2015

 
data_Al(3)Me

_vrf_PLAT601_Al(3)Me
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        109 Ang3  
RESPONSE: There is no residual electron density contained within these 
voids.
;
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C84 H118 Al3 N6 O6' 
_chemical_formula_weight          1388.78

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Al'  'Al'   0.0645   0.0514
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/n'
_space_group_name_Hall            '-P 2yn'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    13.8521(2)
_cell_length_b                    24.7127(3)
_cell_length_c                    22.8860(4)
_cell_angle_alpha                 90
_cell_angle_beta                  93.2630(10)
_cell_angle_gamma                 90
_cell_volume                      7821.7(2)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used   2877
_cell_measurement_theta_min     3.8660
_cell_measurement_theta_max     28.1350
 
_exptl_crystal_density_diffrn     1.179          
_exptl_crystal_F_000              3004
_exptl_crystal_description                'block'
_exptl_crystal_colour                     'clear intense white'
_exptl_crystal_size_max                            0.3500
_exptl_crystal_size_mid                            0.3000
_exptl_crystal_size_min                            0.3000
_exptl_absorpt_coefficient_mu                       0.104
_exptl_absorpt_correction_T_min                   0.97695
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_correction_type            'multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_shelx_estimated_absorpt_T_min    0.979
_shelx_estimated_absorpt_T_max    0.990
_diffrn_ambient_temperature       150(2)
_diffrn_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe 'x-ray'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_monochromator 'graphite'
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'New Xcalibur, EosS2'
_diffrn_detector 'CCD plate'
_diffrn_detector_type 'EosS2'
_diffrn_detector_area_resol_mean 16.1468
_diffrn_reflns_number             61357
_diffrn_reflns_av_unetI/netI      0.0444
_diffrn_reflns_av_R_equivalents   0.0385
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -32
_diffrn_reflns_limit_k_max        30
_diffrn_reflns_limit_l_min        -29
_diffrn_reflns_limit_l_max        25
_diffrn_reflns_theta_min          3.297
_diffrn_reflns_theta_max          27.483
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              17882
_reflns_number_gt                 12764
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
_diffrn_measurement_method 'ω scans'

_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.
;
 
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;

_computing_structure_solution     'SHELXS'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0500P)²+3.2898P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          17882
_refine_ls_number_parameters      908
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0763
_refine_ls_R_factor_gt            0.0477
_refine_ls_wR_factor_ref          0.1224
_refine_ls_wR_factor_gt           0.1079
_refine_ls_goodness_of_fit_ref    1.015
_refine_ls_restrained_S_all       1.015
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
Al1 Al -0.12087(4) 0.14424(2) 0.53906(2) 0.02428(12) Uani 1 1 d . . . . .
O1 O -0.21477(9) 0.19491(5) 0.53731(7) 0.0365(3) Uani 1 1 d . . . . .
N1 N -0.02456(10) 0.20899(6) 0.53070(7) 0.0239(3) Uani 1 1 d . . . . .
C1 C -0.14618(15) 0.10331(9) 0.46655(9) 0.0400(5) Uani 1 1 d . . . . .
H1A H -0.1487 0.0646 0.4756 0.060 Uiso 1 1 calc R U . . .
H1B H -0.0943 0.1101 0.4401 0.060 Uiso 1 1 calc R U . . .
H1C H -0.2082 0.1148 0.4477 0.060 Uiso 1 1 calc R U . . .
Al2 Al 0.28460(3) 0.16979(2) 0.75491(2) 0.02411(12) Uani 1 1 d . . . . .
O2 O -0.16917(9) 0.11286(5) 0.60090(6) 0.0335(3) Uani 1 1 d . . . . .
N2 N 0.02270(10) 0.10641(6) 0.57152(6) 0.0232(3) Uani 1 1 d . . . . .
C2 C -0.21923(12) 0.24420(7) 0.56030(8) 0.0275(4) Uani 1 1 d . . . . .
Al3 Al -0.21558(4) 0.16395(2) 0.85641(2) 0.02283(12) Uani 1 1 d . . . . .
O3 O 0.23144(9) 0.19633(5) 0.68788(6) 0.0308(3) Uani 1 1 d . . . . .
N3 N 0.17428(9) 0.21692(5) 0.80065(6) 0.0221(3) Uani 1 1 d . . . . .
C3 C -0.13554(12) 0.27110(7) 0.58213(8) 0.0270(4) Uani 1 1 d . . . . .
O4 O 0.32679(9) 0.11090(5) 0.71728(6) 0.0348(3) Uani 1 1 d . . . . .
N4 N 0.24419(10) 0.11499(5) 0.81956(6) 0.0231(3) Uani 1 1 d . . . . .
C4 C -0.14211(14) 0.32327(8) 0.60435(9) 0.0321(4) Uani 1 1 d . . . . .
H4 H -0.0848 0.3414 0.6183 0.039 Uiso 1 1 calc R U . . .
O5 O -0.10059(8) 0.13396(5) 0.87015(6) 0.0268(3) Uani 1 1 d . . . . .
N5 N -0.24835(9) 0.08962(6) 0.79702(6) 0.0227(3) Uani 1 1 d . . . . .
C5 C -0.23059(15) 0.34954(8) 0.60664(9) 0.0375(5) Uani 1 1 d . . . . .
O6 O -0.17423(9) 0.22926(5) 0.88317(6) 0.0304(3) Uani 1 1 d . . . . .
N6 N -0.25540(9) 0.19990(5) 0.77714(6) 0.0223(3) Uani 1 1 d . . . . .
C6 C -0.31228(14) 0.32238(8) 0.58484(9) 0.0359(5) Uani 1 1 d . . . . .
H6 H -0.3730 0.3401 0.5856 0.043 Uiso 1 1 calc R U . . .
C7 C -0.30958(13) 0.27063(8) 0.56194(8) 0.0299(4) Uani 1 1 d . . . . .
C8 C -0.40055(13) 0.24173(9) 0.54109(9) 0.0387(5) Uani 1 1 d . . . . .
H8A H -0.3873 0.2187 0.5077 0.058 Uiso 1 1 calc R U . . .
H8B H -0.4503 0.2683 0.5292 0.058 Uiso 1 1 calc R U . . .
H8C H -0.4234 0.2193 0.5728 0.058 Uiso 1 1 calc R U . . .
C9 C -0.23885(18) 0.40477(9) 0.63443(12) 0.0543(6) Uani 1 1 d . . . . .
H9A H -0.2876 0.4262 0.6120 0.081 Uiso 1 1 calc R U . . .
H9B H -0.1762 0.4232 0.6345 0.081 Uiso 1 1 calc R U . . .
H9C H -0.2581 0.4007 0.6747 0.081 Uiso 1 1 calc R U . . .
C10 C -0.03888(12) 0.24286(7) 0.58379(8) 0.0276(4) Uani 1 1 d . . . . .
H10A H 0.0131 0.2704 0.5875 0.033 Uiso 1 1 calc R U . . .
H10B H -0.0329 0.2195 0.6189 0.033 Uiso 1 1 calc R U . . .
C11 C -0.04288(14) 0.24170(8) 0.47630(9) 0.0326(4) Uani 1 1 d . . . . .
H11A H -0.0196 0.2793 0.4824 0.039 Uiso 1 1 calc R U . . .
H11B H -0.1128 0.2426 0.4648 0.039 Uiso 1 1 calc R U . . .
C12 C 0.01252(16) 0.21388(9) 0.42981(9) 0.0421(5) Uani 1 1 d . . . . .
H12A H 0.0433 0.2409 0.4049 0.051 Uiso 1 1 calc R U . . .
H12B H -0.0312 0.1909 0.4047 0.051 Uiso 1 1 calc R U . . .
C13 C 0.08903(14) 0.17930(8) 0.46272(9) 0.0357(4) Uani 1 1 d . . . . .
H13A H 0.1545 0.1889 0.4510 0.043 Uiso 1 1 calc R U . . .
H13B H 0.0776 0.1404 0.4547 0.043 Uiso 1 1 calc R U . . .
C14 C 0.07866(12) 0.19181(7) 0.52779(8) 0.0262(4) Uani 1 1 d . . . . .
H14 H 0.1204 0.2238 0.5382 0.031 Uiso 1 1 calc R U . . .
C15 C 0.10224(11) 0.14771(7) 0.57297(8) 0.0235(4) Uani 1 1 d . . . . .
H15 H 0.1069 0.1647 0.6127 0.028 Uiso 1 1 calc R U . . .
C16 C 0.19710(12) 0.11713(7) 0.56411(9) 0.0308(4) Uani 1 1 d . . . . .
H16A H 0.2348 0.1356 0.5345 0.037 Uiso 1 1 calc R U . . .
H16B H 0.2370 0.1151 0.6013 0.037 Uiso 1 1 calc R U . . .
C17 C 0.16726(14) 0.06020(8) 0.54301(10) 0.0408(5) Uani 1 1 d . . . . .
H17A H 0.1974 0.0513 0.5060 0.049 Uiso 1 1 calc R U . . .
H17B H 0.1873 0.0327 0.5728 0.049 Uiso 1 1 calc R U . . .
C18 C 0.05771(13) 0.06177(7) 0.53368(8) 0.0301(4) Uani 1 1 d . . . . .
H18A H 0.0387 0.0689 0.4920 0.036 Uiso 1 1 calc R U . . .
H18B H 0.0294 0.0267 0.5449 0.036 Uiso 1 1 calc R U . . .
C19 C 0.01648(12) 0.08438(7) 0.63274(8) 0.0260(4) Uani 1 1 d . . . . .
H19A H 0.0789 0.0675 0.6456 0.031 Uiso 1 1 calc R U . . .
H19B H 0.0039 0.1144 0.6599 0.031 Uiso 1 1 calc R U . . .
C20 C -0.06247(12) 0.04337(7) 0.63486(8) 0.0259(4) Uani 1 1 d . . . . .
C21 C -0.15472(13) 0.06068(8) 0.61613(8) 0.0289(4) Uani 1 1 d . . . . .
C22 C -0.23173(13) 0.02371(9) 0.61324(9) 0.0365(5) Uani 1 1 d . . . . .
C23 C -0.21406(16) -0.02870(9) 0.63260(9) 0.0418(5) Uani 1 1 d . . . . .
H23 H -0.2663 -0.0537 0.6313 0.050 Uiso 1 1 calc R U . . .
C24 C -0.12409(16) -0.04637(8) 0.65369(9) 0.0377(5) Uani 1 1 d . . . . .
C25 C -0.04731(14) -0.00991(7) 0.65355(8) 0.0307(4) Uani 1 1 d . . . . .
H25 H 0.0159 -0.0214 0.6663 0.037 Uiso 1 1 calc R U . . .
C26 C -0.32938(15) 0.04188(12) 0.58804(12) 0.0556(7) Uani 1 1 d . . . . .
H26A H -0.3763 0.0125 0.5914 0.083 Uiso 1 1 calc R U . . .
H26B H -0.3247 0.0513 0.5467 0.083 Uiso 1 1 calc R U . . .
H26C H -0.3506 0.0736 0.6096 0.083 Uiso 1 1 calc R U . . .
C27 C -0.1102(2) -0.10358(8) 0.67649(11) 0.0533(6) Uani 1 1 d . . . . .
H27A H -0.1105 -0.1034 0.7193 0.080 Uiso 1 1 calc R U . . .
H27B H -0.0482 -0.1177 0.6645 0.080 Uiso 1 1 calc R U . . .
H27C H -0.1629 -0.1265 0.6604 0.080 Uiso 1 1 calc R U . . .
C28 C 0.40048(13) 0.21158(8) 0.77863(10) 0.0367(5) Uani 1 1 d . . . . .
H28A H 0.4536 0.2011 0.7545 0.055 Uiso 1 1 calc R U . . .
H28B H 0.4188 0.2043 0.8199 0.055 Uiso 1 1 calc R U . . .
H28C H 0.3870 0.2503 0.7734 0.055 Uiso 1 1 calc R U . . .
C29 C 0.20498(12) 0.24800(7) 0.67827(8) 0.0274(4) Uani 1 1 d . . . . .
C30 C 0.13399(12) 0.27081(7) 0.71142(8) 0.0262(4) Uani 1 1 d . . . . .
C31 C 0.10597(13) 0.32438(8) 0.70258(9) 0.0314(4) Uani 1 1 d . . . . .
H31 H 0.0587 0.3397 0.7261 0.038 Uiso 1 1 calc R U . . .
C32 C 0.14605(14) 0.35582(8) 0.65993(9) 0.0356(4) Uani 1 1 d . . . . .
C33 C 0.21534(14) 0.33225(8) 0.62676(9) 0.0369(5) Uani 1 1 d . . . . .
H33 H 0.2424 0.3532 0.5970 0.044 Uiso 1 1 calc R U . . .
C34 C 0.24716(13) 0.27904(9) 0.63519(9) 0.0343(4) Uani 1 1 d . . . . .
C35 C 0.32690(16) 0.25543(10) 0.60100(11) 0.0505(6) Uani 1 1 d . . . . .
H35A H 0.3850 0.2507 0.6269 0.076 Uiso 1 1 calc R U . . .
H35B H 0.3412 0.2800 0.5690 0.076 Uiso 1 1 calc R U . . .
H35C H 0.3063 0.2203 0.5848 0.076 Uiso 1 1 calc R U . . .
C36 C 0.11765(18) 0.41469(9) 0.65164(11) 0.0504(6) Uani 1 1 d . . . . .
H36A H 0.1568 0.4311 0.6220 0.076 Uiso 1 1 calc R U . . .
H36B H 0.1287 0.4341 0.6888 0.076 Uiso 1 1 calc R U . . .
H36C H 0.0491 0.4170 0.6388 0.076 Uiso 1 1 calc R U . . .
C37 C 0.09488(12) 0.23565(7) 0.75781(8) 0.0266(4) Uani 1 1 d . . . . .
H37A H 0.0624 0.2038 0.7393 0.032 Uiso 1 1 calc R U . . .
H37B H 0.0462 0.2561 0.7789 0.032 Uiso 1 1 calc R U . . .
C38 C 0.21467(13) 0.26594(7) 0.83230(9) 0.0288(4) Uani 1 1 d . . . . .
H38A H 0.2200 0.2966 0.8048 0.035 Uiso 1 1 calc R U . . .
H38B H 0.2796 0.2581 0.8506 0.035 Uiso 1 1 calc R U . . .
C39 C 0.14440(15) 0.27958(8) 0.87887(10) 0.0386(5) Uani 1 1 d . . . . .
H39A H 0.0933 0.3045 0.8631 0.046 Uiso 1 1 calc R U . . .
H39B H 0.1786 0.2967 0.9133 0.046 Uiso 1 1 calc R U . . .
C40 C 0.10100(14) 0.22482(7) 0.89551(9) 0.0303(4) Uani 1 1 d . . . . .
H40A H 0.0298 0.2274 0.8964 0.036 Uiso 1 1 calc R U . . .
H40B H 0.1276 0.2130 0.9345 0.036 Uiso 1 1 calc R U . . .
C41 C 0.12940(12) 0.18476(7) 0.84787(8) 0.0228(3) Uani 1 1 d . . . . .
H41 H 0.0694 0.1670 0.8307 0.027 Uiso 1 1 calc R U . . .
C42 C 0.19912(12) 0.14094(7) 0.87032(8) 0.0242(4) Uani 1 1 d . . . . .
H42 H 0.1608 0.1127 0.8900 0.029 Uiso 1 1 calc R U . . .
C43 C 0.28531(14) 0.15641(8) 0.91217(9) 0.0342(4) Uani 1 1 d . . . . .
H43A H 0.3056 0.1942 0.9053 0.041 Uiso 1 1 calc R U . . .
H43B H 0.2684 0.1527 0.9534 0.041 Uiso 1 1 calc R U . . .
C44 C 0.36565(15) 0.11676(9) 0.89828(10) 0.0422(5) Uani 1 1 d . . . . .
H44A H 0.4239 0.1366 0.8870 0.051 Uiso 1 1 calc R U . . .
H44B H 0.3834 0.0939 0.9327 0.051 Uiso 1 1 calc R U . . .
C45 C 0.32488(13) 0.08222(8) 0.84765(9) 0.0315(4) Uani 1 1 d . . . . .
H45A H 0.3750 0.0749 0.8195 0.038 Uiso 1 1 calc R U . . .
H45B H 0.3005 0.0473 0.8621 0.038 Uiso 1 1 calc R U . . .
C46 C 0.17228(12) 0.07980(7) 0.78652(8) 0.0254(4) Uani 1 1 d . . . . .
H46A H 0.1255 0.1030 0.7638 0.030 Uiso 1 1 calc R U . . .
H46B H 0.1359 0.0586 0.8147 0.030 Uiso 1 1 calc R U . . .
C47 C 0.21902(12) 0.04170(7) 0.74564(8) 0.0273(4) Uani 1 1 d . . . . .
C48 C 0.29363(13) 0.06019(8) 0.71195(8) 0.0305(4) Uani 1 1 d . . . . .
C49 C 0.33501(14) 0.02400(9) 0.67296(9) 0.0386(5) Uani 1 1 d . . . . .
C50 C 0.30006(16) -0.02883(9) 0.66925(10) 0.0446(6) Uani 1 1 d . . . . .
H50 H 0.3275 -0.0530 0.6425 0.053 Uiso 1 1 calc R U . . .
C51 C 0.22701(17) -0.04771(8) 0.70292(10) 0.0423(5) Uani 1 1 d . . . . .
C52 C 0.18751(15) -0.01160(7) 0.74111(9) 0.0341(4) Uani 1 1 d . . . . .
H52 H 0.1376 -0.0235 0.7648 0.041 Uiso 1 1 calc R U . . .
C53 C 0.41442(16) 0.04350(11) 0.63589(11) 0.0539(6) Uani 1 1 d . . . . .
H53A H 0.4733 0.0497 0.6608 0.081 Uiso 1 1 calc R U . . .
H53B H 0.3945 0.0774 0.6165 0.081 Uiso 1 1 calc R U . . .
H53C H 0.4270 0.0161 0.6063 0.081 Uiso 1 1 calc R U . . .
C54 C 0.1921(2) -0.10560(9) 0.69956(13) 0.0629(8) Uani 1 1 d . . . . .
H54A H 0.2154 -0.1251 0.7349 0.094 Uiso 1 1 calc R U . . .
H54B H 0.2169 -0.1231 0.6651 0.094 Uiso 1 1 calc R U . . .
H54C H 0.1212 -0.1061 0.6965 0.094 Uiso 1 1 calc R U . . .
C55 C -0.31681(14) 0.15090(8) 0.91152(9) 0.0360(4) Uani 1 1 d . . . . .
H55A H -0.3272 0.1119 0.9154 0.054 Uiso 1 1 calc R U . . .
H55B H -0.3771 0.1682 0.8968 0.054 Uiso 1 1 calc R U . . .
H55C H -0.2967 0.1662 0.9498 0.054 Uiso 1 1 calc R U . . .
C56 C -0.14632(12) 0.27499(7) 0.85827(8) 0.0246(4) Uani 1 1 d . . . . .
C57 C -0.11748(12) 0.31954(7) 0.89399(9) 0.0279(4) Uani 1 1 d . . . . .
C58 C -0.09119(12) 0.36718(7) 0.86736(9) 0.0310(4) Uani 1 1 d . . . . .
H58 H -0.0701 0.3967 0.8914 0.037 Uiso 1 1 calc R U . . .
C59 C -0.09422(13) 0.37378(7) 0.80693(9) 0.0312(4) Uani 1 1 d . . . . .
C60 C -0.12229(12) 0.32945(7) 0.77265(9) 0.0278(4) Uani 1 1 d . . . . .
H60 H -0.1257 0.3330 0.7313 0.033 Uiso 1 1 calc R U . . .
C61 C -0.14562(11) 0.27996(7) 0.79751(8) 0.0239(4) Uani 1 1 d . . . . .
C62 C -0.11510(15) 0.31350(8) 0.95900(9) 0.0371(5) Uani 1 1 d . . . . .
H62A H -0.0961 0.3479 0.9775 0.056 Uiso 1 1 calc R U . . .
H62B H -0.0683 0.2854 0.9713 0.056 Uiso 1 1 calc R U . . .
H62C H -0.1794 0.3032 0.9709 0.056 Uiso 1 1 calc R U . . .
C63 C -0.06851(16) 0.42726(8) 0.77958(11) 0.0450(5) Uani 1 1 d . . . . .
H63A H -0.1138 0.4552 0.7912 0.067 Uiso 1 1 calc R U . . .
H63B H -0.0725 0.4237 0.7369 0.067 Uiso 1 1 calc R U . . .
H63C H -0.0026 0.4375 0.7930 0.067 Uiso 1 1 calc R U . . .
C64 C -0.16742(12) 0.23143(7) 0.75978(8) 0.0237(4) Uani 1 1 d . . . . .
H64A H -0.1105 0.2071 0.7619 0.028 Uiso 1 1 calc R U . . .
H64B H -0.1781 0.2434 0.7186 0.028 Uiso 1 1 calc R U . . .
C65 C -0.33929(12) 0.23848(7) 0.77953(8) 0.0276(4) Uani 1 1 d . . . . .
H65A H -0.3188 0.2727 0.7989 0.033 Uiso 1 1 calc R U . . .
H65B H -0.3921 0.2223 0.8011 0.033 Uiso 1 1 calc R U . . .
C66 C -0.37187(13) 0.24831(8) 0.71594(9) 0.0347(5) Uani 1 1 d . . . . .
H66A H -0.3307 0.2758 0.6981 0.042 Uiso 1 1 calc R U . . .
H66B H -0.4400 0.2605 0.7123 0.042 Uiso 1 1 calc R U . . .
C67 C -0.36020(13) 0.19271(8) 0.68723(9) 0.0339(4) Uani 1 1 d . . . . .
H67A H -0.3376 0.1967 0.6472 0.041 Uiso 1 1 calc R U . . .
H67B H -0.4224 0.1729 0.6850 0.041 Uiso 1 1 calc R U . . .
C68 C -0.28434(12) 0.16244(7) 0.72686(8) 0.0250(4) Uani 1 1 d . . . . .
H68 H -0.2261 0.1561 0.7039 0.030 Uiso 1 1 calc R U . . .
C69 C -0.31767(12) 0.10797(7) 0.74949(8) 0.0250(4) Uani 1 1 d . . . . .
H69 H -0.3179 0.0811 0.7168 0.030 Uiso 1 1 calc R U . . .
C70 C -0.41522(12) 0.10510(7) 0.77780(9) 0.0285(4) Uani 1 1 d . . . . .
H70A H -0.4692 0.1019 0.7477 0.034 Uiso 1 1 calc R U . . .
H70B H -0.4256 0.1375 0.8021 0.034 Uiso 1 1 calc R U . . .
C71 C -0.40640(12) 0.05388(7) 0.81566(9) 0.0309(4) Uani 1 1 d . . . . .
H71A H -0.4398 0.0231 0.7956 0.037 Uiso 1 1 calc R U . . .
H71B H -0.4350 0.0598 0.8538 0.037 Uiso 1 1 calc R U . . .
C72 C -0.29730(12) 0.04283(7) 0.82422(9) 0.0296(4) Uani 1 1 d . . . . .
H72A H -0.2776 0.0402 0.8664 0.035 Uiso 1 1 calc R U . . .
H72B H -0.2804 0.0086 0.8048 0.035 Uiso 1 1 calc R U . . .
C73 C -0.15547(12) 0.07107(7) 0.77373(8) 0.0256(4) Uani 1 1 d . . . . .
H73A H -0.1236 0.1018 0.7549 0.031 Uiso 1 1 calc R U . . .
H73B H -0.1687 0.0427 0.7438 0.031 Uiso 1 1 calc R U . . .
C74 C -0.08979(12) 0.04901(7) 0.82197(8) 0.0253(4) Uani 1 1 d . . . . .
C75 C -0.06808(11) 0.08262(7) 0.87014(8) 0.0241(4) Uani 1 1 d . . . . .
C76 C -0.01150(12) 0.06280(7) 0.91811(8) 0.0274(4) Uani 1 1 d . . . . .
C77 C 0.02458(13) 0.01025(8) 0.91528(9) 0.0309(4) Uani 1 1 d . . . . .
H77 H 0.0637 -0.0032 0.9475 0.037 Uiso 1 1 calc R U . . .
C78 C 0.00581(13) -0.02336(7) 0.86729(9) 0.0309(4) Uani 1 1 d . . . . .
C79 C -0.05292(13) -0.00333(7) 0.82111(9) 0.0292(4) Uani 1 1 d . . . . .
H79 H -0.0683 -0.0258 0.7882 0.035 Uiso 1 1 calc R U . . .
C80 C 0.00717(14) 0.09782(8) 0.97110(9) 0.0347(4) Uani 1 1 d . . . . .
H80A H 0.0511 0.0791 0.9994 0.052 Uiso 1 1 calc R U . . .
H80B H -0.0540 0.1053 0.9890 0.052 Uiso 1 1 calc R U . . .
H80C H 0.0366 0.1320 0.9595 0.052 Uiso 1 1 calc R U . . .
C81 C 0.04770(16) -0.08010(8) 0.86533(11) 0.0437(5) Uani 1 1 d . . . . .
H81A H 0.1169 -0.0780 0.8588 0.066 Uiso 1 1 calc R U . . .
H81B H 0.0147 -0.1005 0.8333 0.066 Uiso 1 1 calc R U . . .
H81C H 0.0385 -0.0985 0.9026 0.066 Uiso 1 1 calc R U . . .
C82 C -0.26924(19) 0.00761(15) 0.99938(13) 0.0812(10) Uani 1 1 d . . . . .
H82A H -0.2675 0.0473 0.9999 0.122 Uiso 1 1 calc R U . . .
H82B H -0.2201 -0.0060 0.9740 0.122 Uiso 1 1 calc R U . . .
H82C H -0.2561 -0.0062 1.0392 0.122 Uiso 1 1 calc R U . . .
C83 C -0.36898(17) -0.01139(12) 0.97614(11) 0.0583(7) Uani 1 1 d . . . . .
H83A H -0.3795 0.0004 0.9349 0.070 Uiso 1 1 calc R U . . .
H83B H -0.3705 -0.0514 0.9767 0.070 Uiso 1 1 calc R U . . .
C84 C -0.45040(16) 0.00973(10) 1.01066(10) 0.0463(5) Uani 1 1 d . . . . .
H84A H -0.4496 0.0498 1.0093 0.056 Uiso 1 1 calc R U . . .
H84B H -0.4386 -0.0012 1.0521 0.056 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Al1 O2 1.7776(14) . ?
Al1 O1 1.8044(13) . ?
Al1 C1 1.958(2) . ?
Al1 N1 2.0989(15) . ?
Al1 N2 2.2831(15) . ?
O1 C2 1.330(2) . ?
N1 C11 1.494(2) . ?
N1 C14 1.497(2) . ?
N1 C10 1.498(2) . ?
Al2 O3 1.7881(14) . ?
Al2 O4 1.8053(14) . ?
Al2 C28 1.9592(19) . ?
Al2 N4 2.1050(15) . ?
Al2 N3 2.2293(15) . ?
O2 C21 1.348(2) . ?
N2 C18 1.500(2) . ?
N2 C15 1.501(2) . ?
N2 C19 1.510(2) . ?
C2 C3 1.403(2) . ?
C2 C7 1.414(2) . ?
Al3 O5 1.7687(12) . ?
Al3 O6 1.8079(13) . ?
Al3 C55 1.9653(19) . ?
Al3 N6 2.0666(15) . ?
Al3 N5 2.3145(15) . ?
O3 C29 1.343(2) . ?
N3 C38 1.503(2) . ?
N3 C37 1.504(2) . ?
N3 C41 1.504(2) . ?
C3 C4 1.391(3) . ?
C3 C10 1.509(2) . ?
O4 C48 1.338(2) . ?
N4 C42 1.494(2) . ?
N4 C46 1.495(2) . ?
N4 C45 1.496(2) . ?
C4 C5 1.391(3) . ?
O5 C75 1.346(2) . ?
N5 C69 1.481(2) . ?
N5 C73 1.493(2) . ?
N5 C72 1.494(2) . ?
C5 C6 1.384(3) . ?
C5 C9 1.513(3) . ?
O6 C56 1.333(2) . ?
N6 C65 1.506(2) . ?
N6 C68 1.513(2) . ?
N6 C64 1.518(2) . ?
C6 C7 1.383(3) . ?
C7 C8 1.502(3) . ?
C11 C12 1.512(3) . ?
C12 C13 1.526(3) . ?
C13 C14 1.536(3) . ?
C14 C15 1.525(2) . ?
C15 C16 1.539(2) . ?
C16 C17 1.537(3) . ?
C17 C18 1.521(3) . ?
C19 C20 1.494(2) . ?
C20 C21 1.392(2) . ?
C20 C25 1.397(3) . ?
C21 C22 1.403(3) . ?
C22 C23 1.386(3) . ?
C22 C26 1.508(3) . ?
C23 C24 1.381(3) . ?
C24 C25 1.394(3) . ?
C24 C27 1.515(3) . ?
C29 C30 1.395(2) . ?
C29 C34 1.403(3) . ?
C30 C31 1.391(3) . ?
C30 C37 1.497(2) . ?
C31 C32 1.388(3) . ?
C32 C33 1.386(3) . ?
C32 C36 1.516(3) . ?
C33 C34 1.397(3) . ?
C34 C35 1.507(3) . ?
C38 C39 1.522(3) . ?
C39 C40 1.537(3) . ?
C40 C41 1.540(2) . ?
C41 C42 1.521(2) . ?
C42 C43 1.536(2) . ?
C43 C44 1.530(3) . ?
C44 C45 1.522(3) . ?
C46 C47 1.500(2) . ?
C47 C52 1.390(3) . ?
C47 C48 1.401(3) . ?
C48 C49 1.408(3) . ?
C49 C50 1.393(3) . ?
C49 C53 1.506(3) . ?
C50 C51 1.387(3) . ?
C51 C52 1.384(3) . ?
C51 C54 1.511(3) . ?
C56 C61 1.397(3) . ?
C56 C57 1.415(2) . ?
C57 C58 1.384(3) . ?
C57 C62 1.494(3) . ?
C58 C59 1.391(3) . ?
C59 C60 1.390(3) . ?
C59 C63 1.514(3) . ?
C60 C61 1.395(2) . ?
C61 C64 1.499(2) . ?
C65 C66 1.519(3) . ?
C66 C67 1.536(3) . ?
C67 C68 1.542(2) . ?
C68 C69 1.523(2) . ?
C69 C70 1.533(2) . ?
C70 C71 1.535(2) . ?
C71 C72 1.537(2) . ?
C73 C74 1.493(2) . ?
C74 C79 1.391(2) . ?
C74 C75 1.399(2) . ?
C75 C76 1.401(2) . ?
C76 C77 1.394(3) . ?
C76 C80 1.500(3) . ?
C77 C78 1.390(3) . ?
C78 C79 1.388(3) . ?
C78 C81 1.519(3) . ?
C82 C83 1.526(4) . ?
C83 C84 1.507(3) . ?
C84 C84 1.510(4) 3_457 ?
 
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
O2 Al1 O1 90.97(7) . . ?
O2 Al1 C1 113.08(8) . . ?
O1 Al1 C1 104.22(8) . . ?
O2 Al1 N1 132.47(7) . . ?
O1 Al1 N1 85.99(6) . . ?
C1 Al1 N1 113.62(8) . . ?
O2 Al1 N2 85.56(6) . . ?
O1 Al1 N2 154.81(6) . . ?
C1 Al1 N2 100.07(7) . . ?
N1 Al1 N2 78.20(5) . . ?
C2 O1 Al1 132.57(11) . . ?
C11 N1 C14 103.52(13) . . ?
C11 N1 C10 110.46(14) . . ?
C14 N1 C10 111.43(13) . . ?
C11 N1 Al1 114.20(11) . . ?
C14 N1 Al1 113.67(10) . . ?
C10 N1 Al1 103.76(10) . . ?
O3 Al2 O4 90.86(6) . . ?
O3 Al2 C28 109.59(8) . . ?
O4 Al2 C28 105.95(8) . . ?
O3 Al2 N4 136.55(6) . . ?
O4 Al2 N4 85.58(6) . . ?
C28 Al2 N4 113.01(8) . . ?
O3 Al2 N3 87.22(6) . . ?
O4 Al2 N3 153.44(6) . . ?
C28 Al2 N3 99.62(7) . . ?
N4 Al2 N3 77.84(5) . . ?
C21 O2 Al1 124.49(12) . . ?
C18 N2 C15 104.59(13) . . ?
C18 N2 C19 107.94(13) . . ?
C15 N2 C19 107.77(13) . . ?
C18 N2 Al1 114.68(11) . . ?
C15 N2 Al1 110.70(10) . . ?
C19 N2 Al1 110.78(10) . . ?
O1 C2 C3 121.26(16) . . ?
O1 C2 C7 119.64(16) . . ?
C3 C2 C7 119.09(17) . . ?
O5 Al3 O6 92.81(6) . . ?
O5 Al3 C55 119.04(8) . . ?
O6 Al3 C55 98.80(8) . . ?
O5 Al3 N6 121.93(6) . . ?
O6 Al3 N6 88.70(6) . . ?
C55 Al3 N6 117.99(8) . . ?
O5 Al3 N5 85.20(5) . . ?
O6 Al3 N5 162.79(6) . . ?
C55 Al3 N5 97.09(7) . . ?
N6 Al3 N5 78.00(5) . . ?
C29 O3 Al2 125.76(12) . . ?
C38 N3 C37 107.73(13) . . ?
C38 N3 C41 103.74(13) . . ?
C37 N3 C41 108.30(12) . . ?
C38 N3 Al2 113.65(10) . . ?
C37 N3 Al2 110.49(11) . . ?
C41 N3 Al2 112.56(10) . . ?
C4 C3 C2 119.96(16) . . ?
C4 C3 C10 119.74(16) . . ?
C2 C3 C10 120.26(16) . . ?
C48 O4 Al2 132.84(12) . . ?
C42 N4 C46 110.30(13) . . ?
C42 N4 C45 103.50(14) . . ?
C46 N4 C45 111.27(13) . . ?
C42 N4 Al2 114.20(10) . . ?
C46 N4 Al2 102.41(11) . . ?
C45 N4 Al2 115.37(11) . . ?
C5 C4 C3 121.51(18) . . ?
C75 O5 Al3 133.84(11) . . ?
C69 N5 C73 111.58(13) . . ?
C69 N5 C72 104.62(13) . . ?
C73 N5 C72 109.39(13) . . ?
C69 N5 Al3 106.60(10) . . ?
C73 N5 Al3 108.01(10) . . ?
C72 N5 Al3 116.62(11) . . ?
C6 C5 C4 117.66(18) . . ?
C6 C5 C9 120.62(19) . . ?
C4 C5 C9 121.7(2) . . ?
C56 O6 Al3 134.92(12) . . ?
C65 N6 C68 104.09(13) . . ?
C65 N6 C64 108.49(12) . . ?
C68 N6 C64 107.27(13) . . ?
C65 N6 Al3 114.08(11) . . ?
C68 N6 Al3 116.77(10) . . ?
C64 N6 Al3 105.79(10) . . ?
C7 C6 C5 123.08(17) . . ?
C6 C7 C2 118.69(17) . . ?
C6 C7 C8 121.30(17) . . ?
C2 C7 C8 119.98(18) . . ?
N1 C10 C3 113.35(15) . . ?
N1 C11 C12 105.75(15) . . ?
C11 C12 C13 105.86(16) . . ?
C12 C13 C14 105.37(16) . . ?
N1 C14 C15 109.93(14) . . ?
N1 C14 C13 104.04(14) . . ?
C15 C14 C13 119.04(15) . . ?
N2 C15 C14 110.02(13) . . ?
N2 C15 C16 107.12(13) . . ?
C14 C15 C16 114.39(15) . . ?
C17 C16 C15 105.93(14) . . ?
C18 C17 C16 105.62(15) . . ?
N2 C18 C17 106.88(14) . . ?
C20 C19 N2 110.80(14) . . ?
C21 C20 C25 120.23(17) . . ?
C21 C20 C19 116.27(16) . . ?
C25 C20 C19 123.50(16) . . ?
O2 C21 C20 119.60(16) . . ?
O2 C21 C22 120.63(17) . . ?
C20 C21 C22 119.78(18) . . ?
C23 C22 C21 118.25(18) . . ?
C23 C22 C26 122.59(19) . . ?
C21 C22 C26 119.1(2) . . ?
C24 C23 C22 123.13(18) . . ?
C23 C24 C25 117.91(19) . . ?
C23 C24 C27 120.64(19) . . ?
C25 C24 C27 121.4(2) . . ?
C24 C25 C20 120.57(18) . . ?
O3 C29 C30 119.30(16) . . ?
O3 C29 C34 120.95(17) . . ?
C30 C29 C34 119.75(17) . . ?
C31 C30 C29 120.33(17) . . ?
C31 C30 C37 123.12(16) . . ?
C29 C30 C37 116.48(16) . . ?
C32 C31 C30 121.03(18) . . ?
C33 C32 C31 117.87(18) . . ?
C33 C32 C36 121.18(19) . . ?
C31 C32 C36 120.91(19) . . ?
C32 C33 C34 122.89(18) . . ?
C33 C34 C29 118.11(18) . . ?
C33 C34 C35 121.85(19) . . ?
C29 C34 C35 120.01(19) . . ?
C30 C37 N3 111.11(13) . . ?
N3 C38 C39 106.30(14) . . ?
C38 C39 C40 104.68(14) . . ?
C39 C40 C41 105.73(15) . . ?
N3 C41 C42 109.79(13) . . ?
N3 C41 C40 107.54(13) . . ?
C42 C41 C40 113.67(15) . . ?
N4 C42 C41 109.17(14) . . ?
N4 C42 C43 104.31(14) . . ?
C41 C42 C43 119.32(15) . . ?
C44 C43 C42 105.07(15) . . ?
C45 C44 C43 105.94(15) . . ?
N4 C45 C44 105.04(15) . . ?
N4 C46 C47 112.44(14) . . ?
C52 C47 C48 120.43(17) . . ?
C52 C47 C46 119.78(17) . . ?
C48 C47 C46 119.79(16) . . ?
O4 C48 C47 121.03(16) . . ?
O4 C48 C49 120.18(18) . . ?
C47 C48 C49 118.78(18) . . ?
C50 C49 C48 118.8(2) . . ?
C50 C49 C53 121.86(19) . . ?
C48 C49 C53 119.4(2) . . ?
C51 C50 C49 122.91(19) . . ?
C52 C51 C50 117.47(19) . . ?
C52 C51 C54 120.4(2) . . ?
C50 C51 C54 122.1(2) . . ?
C51 C52 C47 121.6(2) . . ?
O6 C56 C61 121.26(16) . . ?
O6 C56 C57 119.46(17) . . ?
C61 C56 C57 119.27(16) . . ?
C58 C57 C56 118.70(18) . . ?
C58 C57 C62 122.14(17) . . ?
C56 C57 C62 119.15(17) . . ?
C57 C58 C59 122.94(17) . . ?
C60 C59 C58 117.42(17) . . ?
C60 C59 C63 121.30(19) . . ?
C58 C59 C63 121.28(18) . . ?
C59 C60 C61 121.66(18) . . ?
C60 C61 C56 119.88(16) . . ?
C60 C61 C64 120.70(16) . . ?
C56 C61 C64 119.40(15) . . ?
C61 C64 N6 113.47(14) . . ?
N6 C65 C66 104.73(15) . . ?
C65 C66 C67 103.54(15) . . ?
C66 C67 C68 105.50(15) . . ?
N6 C68 C69 110.75(14) . . ?
N6 C68 C67 107.01(14) . . ?
C69 C68 C67 114.78(14) . . ?
N5 C69 C68 108.91(13) . . ?
N5 C69 C70 103.05(14) . . ?
C68 C69 C70 118.44(15) . . ?
C69 C70 C71 103.47(14) . . ?
C70 C71 C72 105.34(14) . . ?
N5 C72 C71 106.00(14) . . ?
N5 C73 C74 110.45(14) . . ?
C79 C74 C75 120.03(17) . . ?
C79 C74 C73 122.53(17) . . ?
C75 C74 C73 117.40(15) . . ?
O5 C75 C74 120.18(16) . . ?
O5 C75 C76 120.12(16) . . ?
C74 C75 C76 119.70(16) . . ?
C77 C76 C75 118.39(17) . . ?
C77 C76 C80 121.94(17) . . ?
C75 C76 C80 119.66(16) . . ?
C78 C77 C76 122.81(18) . . ?
C79 C78 C77 117.65(17) . . ?
C79 C78 C81 120.99(19) . . ?
C77 C78 C81 121.35(18) . . ?
C78 C79 C74 121.37(18) . . ?
C84 C83 C82 113.6(2) . . ?
C83 C84 C84 114.5(3) . 3_457 ?
 
_refine_diff_density_max    0.265
_refine_diff_density_min   -0.231
_refine_diff_density_rms    0.045

#====END

data_Al(1)Me

_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C27 H37 Al N2 O2' 
_chemical_formula_weight          448.56

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Al'  'Al'   0.0645   0.0514
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            4
_space_group_name_H-M_alt         'P 21'
_space_group_name_Hall            'P 2yb'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z'
 
_cell_length_a                    9.9462(12)
_cell_length_b                    10.3018(11)
_cell_length_c                    12.8708(15)
_cell_angle_alpha                 90
_cell_angle_beta                  108.547(14)
_cell_angle_gamma                 90
_cell_volume                      1250.3(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used   3217
_cell_measurement_theta_min     3.6650
_cell_measurement_theta_max     29.012
_exptl_crystal_description                'block'
_exptl_crystal_colour                     'clear intense yellow'
_exptl_crystal_size_max                            0.3000
_exptl_crystal_size_mid                            0.1000
_exptl_crystal_size_min                            0.0500
_exptl_crystal_density_diffrn     1.191          
_exptl_crystal_F_000              484
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_absorpt_coefficient_mu     0.107
_shelx_estimated_absorpt_T_min    0.969
_shelx_estimated_absorpt_T_max    0.979
_exptl_absorpt_correction_T_min                   0.94819
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_correction_type            'multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature       150(2)
_diffrn_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe 'x-ray'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_monochromator 'graphite'
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'New Xcalibur, EosS2'
_diffrn_detector 'CCD plate'
_diffrn_detector_type 'EosS2'
_diffrn_detector_area_resol_mean 16.1468
_diffrn_reflns_number             10007
_diffrn_reflns_av_unetI/netI      0.0436
_diffrn_reflns_av_R_equivalents   0.0227
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          3.339
_diffrn_reflns_theta_max          27.484
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.997
_diffrn_measured_fraction_theta_full  0.997
_diffrn_reflns_Laue_measured_fraction_max    0.997
_diffrn_reflns_Laue_measured_fraction_full   0.997
_diffrn_reflns_point_group_measured_fraction_max   0.967
_diffrn_reflns_point_group_measured_fraction_full  0.977
_reflns_number_total              5543
_reflns_number_gt                 4958
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.837
_reflns_Friedel_fraction_max      0.933
_reflns_Friedel_fraction_full     0.954
_diffrn_measurement_method 'ω scans'
 
_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.
;
 
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution     'SHELXS'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0334P)²+0.2164P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Flack x determined using 2010 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.01(8)
_chemical_absolute_configuration  ad
_refine_ls_number_reflns          5543
_refine_ls_number_parameters      294
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0463
_refine_ls_R_factor_gt            0.0382
_refine_ls_wR_factor_ref          0.0828
_refine_ls_wR_factor_gt           0.0795
_refine_ls_goodness_of_fit_ref    1.028
_refine_ls_restrained_S_all       1.028
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
Al1 Al 0.80488(7) 0.37431(7) 0.30399(5) 0.01871(16) Uani 1 1 d . . . . .
O1 O 0.8234(2) 0.27109(16) 0.42323(14) 0.0250(4) Uani 1 1 d . . . . .
N1 N 0.7910(2) 0.53624(19) 0.39316(16) 0.0185(4) Uani 1 1 d . . . . .
C1 C 0.9788(3) 0.3102(3) 0.2787(2) 0.0278(6) Uani 1 1 d . . . . .
H1A H 0.9894 0.2171 0.2949 0.042 Uiso 1 1 calc R U . . .
H1B H 1.0611 0.3568 0.3267 0.042 Uiso 1 1 calc R U . . .
H1C H 0.9722 0.3249 0.2020 0.042 Uiso 1 1 calc R U . . .
O2 O 0.63420(18) 0.32251(16) 0.22342(14) 0.0251(4) Uani 1 1 d . . . . .
N2 N 0.7867(2) 0.5379(2) 0.17779(16) 0.0212(4) Uani 1 1 d . . . . .
C2 C 0.8055(3) 0.2946(2) 0.51992(19) 0.0209(5) Uani 1 1 d . . . . .
C3 C 0.7491(3) 0.1999(2) 0.5727(2) 0.0242(5) Uani 1 1 d . . . . .
C4 C 0.7315(3) 0.2301(3) 0.6735(2) 0.0273(6) Uani 1 1 d . . . . .
H4 H 0.6950 0.1653 0.7097 0.033 Uiso 1 1 calc R U . . .
C5 C 0.7653(3) 0.3517(3) 0.7231(2) 0.0297(6) Uani 1 1 d . . . . .
C6 C 0.8216(3) 0.4442(2) 0.6698(2) 0.0256(6) Uani 1 1 d . . . . .
H6 H 0.8458 0.5276 0.7018 0.031 Uiso 1 1 calc R U . . .
C7 C 0.8432(3) 0.4165(2) 0.57035(19) 0.0215(5) Uani 1 1 d . . . . .
C8 C 0.7039(3) 0.0704(3) 0.5187(3) 0.0337(6) Uani 1 1 d . . . . .
H8A H 0.6236 0.0825 0.4516 0.051 Uiso 1 1 calc R U . . .
H8B H 0.6756 0.0132 0.5689 0.051 Uiso 1 1 calc R U . . .
H8C H 0.7832 0.0310 0.5003 0.051 Uiso 1 1 calc R U . . .
C9 C 0.7366(4) 0.3831(4) 0.8293(2) 0.0443(8) Uani 1 1 d . . . . .
H9A H 0.7222 0.3023 0.8646 0.066 Uiso 1 1 calc R U . . .
H9B H 0.6514 0.4371 0.8136 0.066 Uiso 1 1 calc R U . . .
H9C H 0.8178 0.4302 0.8783 0.066 Uiso 1 1 calc R U . . .
C10 C 0.8959(3) 0.5171(2) 0.50815(19) 0.0216(5) Uani 1 1 d . . . . .
H10A H 0.9888 0.4895 0.5026 0.026 Uiso 1 1 calc R U . . .
H10B H 0.9096 0.6004 0.5484 0.026 Uiso 1 1 calc R U . . .
C11 C 0.6461(3) 0.5652(2) 0.4011(2) 0.0217(5) Uani 1 1 d . . . . .
H11A H 0.6229 0.5051 0.4530 0.026 Uiso 1 1 calc R U . . .
H11B H 0.5726 0.5572 0.3286 0.026 Uiso 1 1 calc R U . . .
C12 C 0.6558(3) 0.7055(3) 0.4430(2) 0.0333(7) Uani 1 1 d . . . . .
H12A H 0.5638 0.7506 0.4121 0.040 Uiso 1 1 calc R U . . .
H12B H 0.6829 0.7073 0.5240 0.040 Uiso 1 1 calc R U . . .
C13 C 0.7704(3) 0.7702(2) 0.4043(2) 0.0302(6) Uani 1 1 d . . . . .
H13A H 0.8476 0.8052 0.4672 0.036 Uiso 1 1 calc R U . . .
H13B H 0.7297 0.8418 0.3525 0.036 Uiso 1 1 calc R U . . .
C14 C 0.8258(3) 0.6612(2) 0.3472(2) 0.0221(5) Uani 1 1 d . . . . .
H14 H 0.9307 0.6694 0.3635 0.026 Uiso 1 1 calc R U . . .
C15 C 0.7508(3) 0.6621(2) 0.2226(2) 0.0225(5) Uani 1 1 d . . . . .
H15 H 0.6459 0.6682 0.2070 0.027 Uiso 1 1 calc R U . . .
C16 C 0.8020(4) 0.7741(3) 0.1649(2) 0.0373(7) Uani 1 1 d . . . . .
H16A H 0.7206 0.8168 0.1103 0.045 Uiso 1 1 calc R U . . .
H16B H 0.8541 0.8398 0.2189 0.045 Uiso 1 1 calc R U . . .
C17 C 0.8996(3) 0.7111(3) 0.1089(2) 0.0359(7) Uani 1 1 d . . . . .
H17A H 0.9916 0.7572 0.1278 0.043 Uiso 1 1 calc R U . . .
H17B H 0.8554 0.7112 0.0283 0.043 Uiso 1 1 calc R U . . .
C18 C 0.9197(3) 0.5717(3) 0.1538(2) 0.0284(6) Uani 1 1 d . . . . .
H18A H 0.9351 0.5113 0.0989 0.034 Uiso 1 1 calc R U . . .
H18B H 1.0024 0.5668 0.2213 0.034 Uiso 1 1 calc R U . . .
C19 C 0.6757(3) 0.5013(3) 0.0719(2) 0.0244(6) Uani 1 1 d . . . . .
H19A H 0.6689 0.5709 0.0175 0.029 Uiso 1 1 calc R U . . .
H19B H 0.7057 0.4208 0.0434 0.029 Uiso 1 1 calc R U . . .
C20 C 0.5322(3) 0.4800(2) 0.08366(19) 0.0215(5) Uani 1 1 d . . . . .
C21 C 0.4129(3) 0.5469(3) 0.0197(2) 0.0247(5) Uani 1 1 d . . . . .
H21 H 0.4227 0.6093 -0.0317 0.030 Uiso 1 1 calc R U . . .
C22 C 0.2800(3) 0.5244(3) 0.0296(2) 0.0276(6) Uani 1 1 d . . . . .
C23 C 0.2704(3) 0.4334(3) 0.1071(2) 0.0278(6) Uani 1 1 d . . . . .
H23 H 0.1803 0.4174 0.1154 0.033 Uiso 1 1 calc R U . . .
C24 C 0.3872(3) 0.3648(3) 0.17302(19) 0.0251(5) Uani 1 1 d . . . . .
C25 C 0.5203(2) 0.3881(2) 0.16066(18) 0.0206(5) Uani 1 1 d . . . . .
C26 C 0.1500(3) 0.5927(3) -0.0443(3) 0.0395(7) Uani 1 1 d . . . . .
H26A H 0.0817 0.5281 -0.0861 0.059 Uiso 1 1 calc R U . . .
H26B H 0.1776 0.6498 -0.0950 0.059 Uiso 1 1 calc R U . . .
H26C H 0.1064 0.6445 0.0003 0.059 Uiso 1 1 calc R U . . .
C27 C 0.3759(3) 0.2671(3) 0.2572(3) 0.0378(7) Uani 1 1 d . . . . .
H27A H 0.2763 0.2575 0.2531 0.057 Uiso 1 1 calc R U . . .
H27B H 0.4314 0.2971 0.3305 0.057 Uiso 1 1 calc R U . . .
H27C H 0.4126 0.1831 0.2425 0.057 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Al1 O2 1.7669(18) . ?
Al1 O1 1.8276(19) . ?
Al1 C1 1.973(3) . ?
Al1 N1 2.054(2) . ?
Al1 N2 2.307(2) . ?
O1 C2 1.334(3) . ?
N1 C14 1.502(3) . ?
N1 C11 1.507(3) . ?
N1 C10 1.528(3) . ?
O2 C25 1.345(3) . ?
N2 C18 1.492(3) . ?
N2 C15 1.493(3) . ?
N2 C19 1.504(3) . ?
C2 C3 1.404(3) . ?
C2 C7 1.409(3) . ?
C3 C4 1.397(4) . ?
C3 C8 1.506(4) . ?
C4 C5 1.398(4) . ?
C5 C6 1.391(4) . ?
C5 C9 1.518(4) . ?
C6 C7 1.394(3) . ?
C7 C10 1.502(3) . ?
C11 C12 1.535(4) . ?
C12 C13 1.534(4) . ?
C13 C14 1.537(4) . ?
C14 C15 1.539(3) . ?
C15 C16 1.543(4) . ?
C16 C17 1.527(4) . ?
C17 C18 1.536(4) . ?
C19 C20 1.498(4) . ?
C20 C21 1.393(3) . ?
C20 C25 1.403(3) . ?
C21 C22 1.387(4) . ?
C22 C23 1.394(4) . ?
C22 C26 1.514(4) . ?
C23 C24 1.393(4) . ?
C24 C25 1.404(3) . ?
C24 C27 1.509(4) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O2 Al1 O1 97.97(9) . . ?
O2 Al1 C1 122.09(11) . . ?
O1 Al1 C1 94.82(10) . . ?
O2 Al1 N1 110.51(9) . . ?
O1 Al1 N1 90.58(8) . . ?
C1 Al1 N1 125.61(11) . . ?
O2 Al1 N2 87.82(8) . . ?
O1 Al1 N2 168.66(8) . . ?
C1 Al1 N2 90.28(10) . . ?
N1 Al1 N2 78.24(8) . . ?
C2 O1 Al1 132.05(16) . . ?
C14 N1 C11 101.67(18) . . ?
C14 N1 C10 108.68(18) . . ?
C11 N1 C10 109.44(18) . . ?
C14 N1 Al1 114.26(15) . . ?
C11 N1 Al1 115.77(14) . . ?
C10 N1 Al1 106.83(14) . . ?
C25 O2 Al1 131.98(15) . . ?
C18 N2 C15 102.5(2) . . ?
C18 N2 C19 108.35(19) . . ?
C15 N2 C19 111.59(19) . . ?
C18 N2 Al1 116.13(15) . . ?
C15 N2 Al1 109.20(14) . . ?
C19 N2 Al1 108.99(15) . . ?
O1 C2 C3 121.2(2) . . ?
O1 C2 C7 119.7(2) . . ?
C3 C2 C7 119.0(2) . . ?
C4 C3 C2 118.8(2) . . ?
C4 C3 C8 121.3(2) . . ?
C2 C3 C8 119.9(2) . . ?
C3 C4 C5 122.7(2) . . ?
C6 C5 C4 117.7(2) . . ?
C6 C5 C9 121.2(3) . . ?
C4 C5 C9 121.0(3) . . ?
C5 C6 C7 121.1(2) . . ?
C6 C7 C2 120.6(2) . . ?
C6 C7 C10 122.1(2) . . ?
C2 C7 C10 117.2(2) . . ?
C7 C10 N1 111.03(19) . . ?
N1 C11 C12 104.8(2) . . ?
C13 C12 C11 105.4(2) . . ?
C12 C13 C14 104.7(2) . . ?
N1 C14 C13 106.0(2) . . ?
N1 C14 C15 108.65(19) . . ?
C13 C14 C15 111.4(2) . . ?
N2 C15 C14 107.53(19) . . ?
N2 C15 C16 107.4(2) . . ?
C14 C15 C16 112.4(2) . . ?
C17 C16 C15 105.4(2) . . ?
C16 C17 C18 104.2(2) . . ?
N2 C18 C17 106.2(2) . . ?
C20 C19 N2 113.2(2) . . ?
C21 C20 C25 120.3(2) . . ?
C21 C20 C19 121.9(2) . . ?
C25 C20 C19 117.8(2) . . ?
C22 C21 C20 121.4(2) . . ?
C21 C22 C23 117.6(2) . . ?
C21 C22 C26 120.9(3) . . ?
C23 C22 C26 121.6(3) . . ?
C24 C23 C22 122.9(3) . . ?
C23 C24 C25 118.6(2) . . ?
C23 C24 C27 122.5(2) . . ?
C25 C24 C27 118.9(2) . . ?
O2 C25 C20 121.3(2) . . ?
O2 C25 C24 119.4(2) . . ?
C20 C25 C24 119.4(2) . . ?
 
_refine_diff_density_max    0.211
_refine_diff_density_min   -0.179
_refine_diff_density_rms    0.037

#===END

data_Al(1)(OiPr)

# start Validation Reply Form
_vrf_PLAT410_Al(1)(OiPr)
;
PROBLEM: Short Intra H...H Contact  H18B   ..  H19D    ..       1.77 Ang.  
RESPONSE: This is a consequence of the disorder of atom C19.
;
# end Validation Reply Form
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C29 H41 Al N2 O3' 
_chemical_formula_weight          492.62

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Al'  'Al'   0.0645   0.0514
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            19
_space_group_name_H-M_alt         'P 21 21 21'
_space_group_name_Hall            'P 2ac 2ab'
 
_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.
;
 
loop_
 _space_group_symop_operation_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'
 
_cell_length_a                    8.0191(2)
_cell_length_b                    13.4769(3)
_cell_length_c                    25.3790(8)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      2742.77(13)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used   10387
_cell_measurement_theta_min     3.8580
_cell_measurement_theta_max     29.2690
 
_exptl_crystal_description                'block'
_exptl_crystal_colour                     'clear light colourless'
_exptl_crystal_size_max                            0.3000
_exptl_crystal_size_mid                            0.2000
_exptl_crystal_size_min                            0.1000
_exptl_crystal_density_diffrn     1.193          
_exptl_crystal_F_000              1064
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_absorpt_coefficient_mu     0.106
_shelx_estimated_absorpt_T_min    0.969
_shelx_estimated_absorpt_T_max    0.990
_exptl_absorpt_correction_T_min                   0.93608
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_correction_type            'multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature       150(2)
_diffrn_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe 'x-ray'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_monochromator 'graphite'
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'New Xcalibur, EosS2'
_diffrn_detector 'CCD plate'
_diffrn_detector_type 'EosS2'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_reflns_number             27149
_diffrn_reflns_av_unetI/netI      0.0331
_diffrn_reflns_av_R_equivalents   0.0328
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -32
_diffrn_reflns_limit_l_max        32
_diffrn_reflns_theta_min          3.549
_diffrn_reflns_theta_max          27.482
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.995
_diffrn_measured_fraction_theta_full  0.994
_diffrn_reflns_Laue_measured_fraction_max    0.995
_diffrn_reflns_Laue_measured_fraction_full   0.994
_diffrn_reflns_point_group_measured_fraction_max   0.997
_diffrn_reflns_point_group_measured_fraction_full  0.996
_reflns_number_total              6283
_reflns_number_gt                 5754
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.769
_reflns_Friedel_fraction_max      0.999
_reflns_Friedel_fraction_full     0.999
_diffrn_measurement_method 'ω scans'
 
_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.
;
 
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution     SHELXS
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           
;
Atom C19 is disordered over two positions labelled A and B.  The
occupancy was allowed to freely refined and then fixed at the 
converged values of 65:35.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0503P)²+0.4523P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Flack x determined using 2268 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    -0.01(5)
_chemical_absolute_configuration  ad
_refine_ls_number_reflns          6283
_refine_ls_number_parameters      332
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0442
_refine_ls_R_factor_gt            0.0388
_refine_ls_wR_factor_ref          0.0945
_refine_ls_wR_factor_gt           0.0923
_refine_ls_goodness_of_fit_ref    1.055
_refine_ls_restrained_S_all       1.055
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
Al1 Al 0.78797(8) 0.12187(4) 0.35877(3) 0.01608(15) Uani 1 1 d . . . . .
O1 O 0.8365(2) 0.12720(12) 0.29195(6) 0.0246(4) Uani 1 1 d . . . . .
N1 N 0.6657(2) -0.01341(13) 0.34001(7) 0.0181(4) Uani 1 1 d . . . . .
C1 C 0.9351(3) 0.19789(18) 0.26505(10) 0.0263(5) Uani 1 1 d . . . . .
H1 H 0.9102 0.2652 0.2796 0.032 Uiso 1 1 calc R U . . .
O2 O 0.8978(2) 0.06179(11) 0.40952(6) 0.0200(3) Uani 1 1 d . . . . .
N2 N 0.5567(2) 0.15774(12) 0.38411(7) 0.0162(4) Uani 1 1 d . . . . .
C2 C 0.8894(4) 0.1966(2) 0.20725(10) 0.0334(6) Uani 1 1 d . . . . .
H2A H 0.9055 0.1296 0.1931 0.050 Uiso 1 1 calc R U . . .
H2B H 0.9606 0.2433 0.1881 0.050 Uiso 1 1 calc R U . . .
H2C H 0.7723 0.2160 0.2031 0.050 Uiso 1 1 calc R U . . .
O3 O 0.85782(19) 0.24354(11) 0.37888(7) 0.0209(3) Uani 1 1 d . . . . .
C3 C 1.1179(4) 0.1759(3) 0.27326(14) 0.0533(9) Uani 1 1 d . . . . .
H3A H 1.1445 0.1806 0.3109 0.080 Uiso 1 1 calc R U . . .
H3B H 1.1851 0.2240 0.2536 0.080 Uiso 1 1 calc R U . . .
H3C H 1.1427 0.1087 0.2606 0.080 Uiso 1 1 calc R U . . .
C4 C 0.9000(3) -0.03003(16) 0.42975(9) 0.0180(4) Uani 1 1 d . . . . .
C5 C 0.9523(3) -0.04338(17) 0.48211(9) 0.0219(5) Uani 1 1 d . . . . .
C6 C 0.9622(3) -0.13936(19) 0.50198(10) 0.0292(6) Uani 1 1 d . . . . .
H6 H 0.9992 -0.1486 0.5372 0.035 Uiso 1 1 calc R U . . .
C7 C 0.9201(3) -0.22246(18) 0.47218(10) 0.0297(6) Uani 1 1 d . . . . .
C8 C 0.8612(3) -0.20688(16) 0.42148(10) 0.0243(5) Uani 1 1 d . . . . .
H8 H 0.8262 -0.2621 0.4010 0.029 Uiso 1 1 calc R U . . .
C9 C 0.8522(3) -0.11207(16) 0.39998(8) 0.0189(4) Uani 1 1 d . . . . .
C10 C 0.9920(3) 0.04540(18) 0.51594(10) 0.0287(6) Uani 1 1 d . . . . .
H10A H 0.9007 0.0566 0.5409 0.043 Uiso 1 1 calc R U . . .
H10B H 1.0055 0.1041 0.4935 0.043 Uiso 1 1 calc R U . . .
H10C H 1.0956 0.0332 0.5354 0.043 Uiso 1 1 calc R U . . .
C11 C 0.9344(5) -0.3265(2) 0.49514(13) 0.0476(8) Uani 1 1 d . . . . .
H11A H 1.0502 -0.3391 0.5055 0.071 Uiso 1 1 calc R U . . .
H11B H 0.9000 -0.3752 0.4686 0.071 Uiso 1 1 calc R U . . .
H11C H 0.8621 -0.3320 0.5261 0.071 Uiso 1 1 calc R U . . .
C12 C 0.7907(3) -0.09610(15) 0.34463(8) 0.0207(4) Uani 1 1 d . . . . .
H12A H 0.8871 -0.0811 0.3216 0.025 Uiso 1 1 calc R U . . .
H12B H 0.7391 -0.1583 0.3318 0.025 Uiso 1 1 calc R U . . .
C13 C 0.5863(3) -0.02160(17) 0.28666(9) 0.0250(5) Uani 1 1 d . . . . .
H13A H 0.6685 -0.0448 0.2603 0.030 Uiso 1 1 calc R U . . .
H13B H 0.5421 0.0436 0.2753 0.030 Uiso 1 1 calc R U . . .
C14 C 0.4437(4) -0.09729(18) 0.29249(10) 0.0325(6) Uani 1 1 d . . . . .
H14A H 0.4769 -0.1624 0.2778 0.039 Uiso 1 1 calc R U . . .
H14B H 0.3426 -0.0740 0.2739 0.039 Uiso 1 1 calc R U . . .
C15 C 0.4107(3) -0.10562(16) 0.35237(10) 0.0267(5) Uani 1 1 d . . . . .
H15A H 0.2918 -0.0932 0.3605 0.032 Uiso 1 1 calc R U . . .
H15B H 0.4420 -0.1721 0.3657 0.032 Uiso 1 1 calc R U . . .
C16 C 0.5222(3) -0.02493(15) 0.37644(9) 0.0192(4) Uani 1 1 d . . . . .
H16 H 0.5616 -0.0454 0.4122 0.023 Uiso 1 1 calc R U . . .
C17 C 0.4316(3) 0.07442(15) 0.37932(9) 0.0200(4) Uani 1 1 d . . . . .
H17 H 0.3648 0.0839 0.3464 0.024 Uiso 1 1 calc R U . . .
C18 C 0.3157(3) 0.08305(18) 0.42716(11) 0.0286(5) Uani 1 1 d . . . . .
H18A H 0.1987 0.0917 0.4156 0.034 Uiso 1 1 calc R U . A 1
H18B H 0.3230 0.0226 0.4492 0.034 Uiso 1 1 calc R U . A 1
C19A C 0.3741(5) 0.1737(3) 0.45819(16) 0.0299(8) Uani 0.65 1 d . . P B 1
H19A H 0.3079 0.2332 0.4488 0.036 Uiso 0.65 1 calc R U P B 1
H19B H 0.3651 0.1621 0.4966 0.036 Uiso 0.65 1 calc R U P B 1
C20 C 0.5544(3) 0.18569(17) 0.44171(9) 0.0218(5) Uani 1 1 d . . . . .
H20A H 0.5919 0.2550 0.4467 0.026 Uiso 1 1 calc R U . B 1
H20B H 0.6276 0.1412 0.4624 0.026 Uiso 1 1 calc R U . B 1
C21 C 0.5032(3) 0.24341(15) 0.35029(9) 0.0198(5) Uani 1 1 d . . . . .
H21A H 0.3866 0.2608 0.3592 0.024 Uiso 1 1 calc R U . . .
H21B H 0.5052 0.2222 0.3129 0.024 Uiso 1 1 calc R U . . .
C22 C 0.6106(3) 0.33518(15) 0.35619(9) 0.0178(4) Uani 1 1 d . . . . .
C23 C 0.7806(3) 0.32943(14) 0.36915(8) 0.0178(4) Uani 1 1 d . . . . .
C24 C 0.8729(3) 0.41870(16) 0.37272(9) 0.0226(5) Uani 1 1 d . . . . .
C25 C 0.7953(3) 0.50816(15) 0.36235(10) 0.0238(5) Uani 1 1 d . . . . .
H25 H 0.8589 0.5675 0.3644 0.029 Uiso 1 1 calc R U . . .
C26 C 0.6271(3) 0.51466(15) 0.34897(9) 0.0209(5) Uani 1 1 d . . . . .
C27 C 0.5372(3) 0.42688(16) 0.34661(8) 0.0195(4) Uani 1 1 d . . . . .
H27 H 0.4218 0.4295 0.3382 0.023 Uiso 1 1 calc R U . . .
C28 C 1.0555(3) 0.41293(19) 0.38633(14) 0.0386(7) Uani 1 1 d . . . . .
H28A H 1.1160 0.3806 0.3575 0.058 Uiso 1 1 calc R U . . .
H28B H 1.0698 0.3744 0.4188 0.058 Uiso 1 1 calc R U . . .
H28C H 1.0995 0.4801 0.3915 0.058 Uiso 1 1 calc R U . . .
C29 C 0.5443(4) 0.61345(16) 0.33844(10) 0.0289(5) Uani 1 1 d . . . . .
H29A H 0.5721 0.6599 0.3668 0.043 Uiso 1 1 calc R U . . .
H29B H 0.4232 0.6044 0.3369 0.043 Uiso 1 1 calc R U . . .
H29C H 0.5840 0.6400 0.3048 0.043 Uiso 1 1 calc R U . . .
C19B C 0.4446(10) 0.1136(5) 0.4700(3) 0.0267(15) Uani 0.35 1 d . . P B 2
H19C H 0.3889 0.1454 0.5005 0.032 Uiso 0.35 1 calc R U P B 2
H19D H 0.5089 0.0555 0.4825 0.032 Uiso 0.35 1 calc R U P B 2
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Al1 O1 1.7414(17) . ?
Al1 O2 1.7579(16) . ?
Al1 O3 1.8063(16) . ?
Al1 N2 2.022(2) . ?
Al1 N1 2.1241(19) . ?
O1 C1 1.414(3) . ?
N1 C16 1.484(3) . ?
N1 C13 1.501(3) . ?
N1 C12 1.503(3) . ?
C1 C3 1.510(4) . ?
C1 C2 1.512(3) . ?
O2 C4 1.340(3) . ?
N2 C21 1.501(3) . ?
N2 C20 1.510(3) . ?
N2 C17 1.511(3) . ?
O3 C23 1.336(2) . ?
C4 C9 1.393(3) . ?
C4 C5 1.405(3) . ?
C5 C6 1.391(3) . ?
C5 C10 1.507(3) . ?
C6 C7 1.393(4) . ?
C7 C8 1.387(3) . ?
C7 C11 1.522(3) . ?
C8 C9 1.391(3) . ?
C9 C12 1.504(3) . ?
C13 C14 1.539(3) . ?
C14 C15 1.547(3) . ?
C15 C16 1.534(3) . ?
C16 C17 1.525(3) . ?
C17 C18 1.533(3) . ?
C18 C19A 1.527(5) . ?
C18 C19B 1.555(8) . ?
C19A C20 1.514(5) . ?
C20 C19B 1.494(7) . ?
C21 C22 1.515(3) . ?
C22 C27 1.390(3) . ?
C22 C23 1.405(3) . ?
C23 C24 1.415(3) . ?
C24 C25 1.382(3) . ?
C24 C28 1.506(3) . ?
C25 C26 1.393(3) . ?
C26 C27 1.387(3) . ?
C26 C29 1.511(3) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 Al1 O2 128.36(9) . . ?
O1 Al1 O3 99.70(8) . . ?
O2 Al1 O3 93.19(8) . . ?
O1 Al1 N2 120.32(8) . . ?
O2 Al1 N2 109.67(8) . . ?
O3 Al1 N2 88.72(7) . . ?
O1 Al1 N1 85.43(7) . . ?
O2 Al1 N1 90.00(7) . . ?
O3 Al1 N1 170.27(8) . . ?
N2 Al1 N1 81.55(7) . . ?
C1 O1 Al1 128.53(15) . . ?
C16 N1 C13 103.01(18) . . ?
C16 N1 C12 113.00(17) . . ?
C13 N1 C12 107.39(17) . . ?
C16 N1 Al1 107.95(13) . . ?
C13 N1 Al1 117.47(13) . . ?
C12 N1 Al1 108.13(14) . . ?
O1 C1 C3 110.1(2) . . ?
O1 C1 C2 109.0(2) . . ?
C3 C1 C2 111.5(2) . . ?
C4 O2 Al1 135.46(15) . . ?
C21 N2 C20 110.99(16) . . ?
C21 N2 C17 109.63(16) . . ?
C20 N2 C17 104.79(16) . . ?
C21 N2 Al1 105.31(13) . . ?
C20 N2 Al1 112.26(14) . . ?
C17 N2 Al1 113.95(13) . . ?
C23 O3 Al1 126.21(14) . . ?
O2 C4 C9 121.45(19) . . ?
O2 C4 C5 119.0(2) . . ?
C9 C4 C5 119.56(19) . . ?
C6 C5 C4 118.6(2) . . ?
C6 C5 C10 121.3(2) . . ?
C4 C5 C10 120.0(2) . . ?
C5 C6 C7 122.5(2) . . ?
C8 C7 C6 117.7(2) . . ?
C8 C7 C11 121.4(2) . . ?
C6 C7 C11 120.9(2) . . ?
C7 C8 C9 121.4(2) . . ?
C8 C9 C4 120.1(2) . . ?
C8 C9 C12 121.0(2) . . ?
C4 C9 C12 118.88(19) . . ?
N1 C12 C9 113.43(17) . . ?
N1 C13 C14 106.09(18) . . ?
C13 C14 C15 105.65(19) . . ?
C16 C15 C14 103.89(18) . . ?
N1 C16 C17 107.90(17) . . ?
N1 C16 C15 106.13(18) . . ?
C17 C16 C15 111.33(19) . . ?
N2 C17 C16 109.87(17) . . ?
N2 C17 C18 106.40(18) . . ?
C16 C17 C18 113.16(18) . . ?
C19A C18 C17 106.5(2) . . ?
C17 C18 C19B 99.8(3) . . ?
C20 C19A C18 103.6(3) . . ?
C19B C20 N2 108.1(3) . . ?
N2 C20 C19A 104.6(2) . . ?
N2 C21 C22 114.14(17) . . ?
C27 C22 C23 120.07(19) . . ?
C27 C22 C21 117.87(19) . . ?
C23 C22 C21 122.02(18) . . ?
O3 C23 C22 122.74(19) . . ?
O3 C23 C24 118.8(2) . . ?
C22 C23 C24 118.40(19) . . ?
C25 C24 C23 119.6(2) . . ?
C25 C24 C28 121.8(2) . . ?
C23 C24 C28 118.6(2) . . ?
C24 C25 C26 122.5(2) . . ?
C27 C26 C25 117.4(2) . . ?
C27 C26 C29 121.0(2) . . ?
C25 C26 C29 121.6(2) . . ?
C26 C27 C22 122.0(2) . . ?
C20 C19B C18 103.2(4) . . ?
 
_refine_diff_density_max    0.233
_refine_diff_density_min   -0.208
_refine_diff_density_rms    0.040

#===END


data_Al(4)(OiPr)
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C41 H65 Al N2 O3' 
_chemical_formula_weight          660.93

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Al'  'Al'   0.0645   0.0514
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    16.6845(10)
_cell_length_b                    19.6643(10)
_cell_length_c                    12.0401(7)
_cell_angle_alpha                 90
_cell_angle_beta                  99.106(6)
_cell_angle_gamma                 90
_cell_volume                      3900.4(4)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used   2631
_cell_measurement_theta_min     3.6830
_cell_measurement_theta_max     24.0390

 
_exptl_crystal_description                'block'
_exptl_crystal_colour                     'clear intense colourless'
_exptl_crystal_size_max                            0.2000
_exptl_crystal_size_mid                            0.1000
_exptl_crystal_size_min                            0.0500

_exptl_crystal_density_diffrn     1.126          
_exptl_crystal_F_000              1448
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_absorpt_coefficient_mu     0.090
_shelx_estimated_absorpt_T_min    0.982
_shelx_estimated_absorpt_T_max    0.996
_exptl_absorpt_correction_T_min                   0.61290
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_correction_type            'multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature       150(2)
_diffrn_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe 'x-ray'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_monochromator 'graphite'
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'New Xcalibur, EosS2'
_diffrn_detector 'CCD plate'
_diffrn_detector_type 'EosS2'
_diffrn_detector_area_resol_mean 16.1468
_diffrn_reflns_number             30958
_diffrn_reflns_av_unetI/netI      0.1331
_diffrn_reflns_av_R_equivalents   0.1723
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        19
_diffrn_reflns_limit_k_min        -23
_diffrn_reflns_limit_k_max        23
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          3.345
_diffrn_reflns_theta_max          25.027
_diffrn_reflns_theta_full         25.027
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              6882
_reflns_number_gt                 4075
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
_diffrn_measurement_method 'ω scans'
 
_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.
;
 
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution     SHELXS
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0667P)²+0.1577P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      difmap
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          6882
_refine_ls_number_parameters      438
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1342
_refine_ls_R_factor_gt            0.0773
_refine_ls_wR_factor_ref          0.2001
_refine_ls_wR_factor_gt           0.1651
_refine_ls_goodness_of_fit_ref    1.052
_refine_ls_restrained_S_all       1.052
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
Al1 Al 0.75303(6) 0.59326(5) 0.92531(8) 0.0244(3) Uani 1 1 d . . . . .
O1 O 0.77940(14) 0.51218(12) 0.97002(19) 0.0333(6) Uani 1 1 d . . . . .
N1 N 0.87813(17) 0.62723(14) 1.0042(2) 0.0250(7) Uani 1 1 d . . . . .
C1 C 0.7388(2) 0.45057(18) 0.9420(3) 0.0361(10) Uani 1 1 d . . . . .
H1 H 0.7011 0.4565 0.8693 0.043 Uiso 1 1 calc R U . . .
O2 O 0.77844(13) 0.62232(12) 0.79717(18) 0.0271(6) Uani 1 1 d . . . . .
N2 N 0.72534(17) 0.65670(14) 1.0458(2) 0.0244(7) Uani 1 1 d . . . . .
C2 C 0.6898(2) 0.4317(2) 1.0326(3) 0.0455(11) Uani 1 1 d . . . . .
H2A H 0.7264 0.4255 1.1040 0.068 Uiso 1 1 calc R U . . .
H2B H 0.6604 0.3892 1.0120 0.068 Uiso 1 1 calc R U . . .
H2C H 0.6510 0.4680 1.0406 0.068 Uiso 1 1 calc R U . . .
O3 O 0.64646(13) 0.58653(11) 0.87237(18) 0.0254(6) Uani 1 1 d . . . . .
C3 C 0.8005(3) 0.3969(2) 0.9269(4) 0.0503(12) Uani 1 1 d . . . . .
H3A H 0.8339 0.4126 0.8719 0.075 Uiso 1 1 calc R U . . .
H3B H 0.7726 0.3548 0.9000 0.075 Uiso 1 1 calc R U . . .
H3C H 0.8353 0.3885 0.9991 0.075 Uiso 1 1 calc R U . . .
C4 C 0.8484(2) 0.62901(17) 0.7558(3) 0.0245(8) Uani 1 1 d . . . . .
C5 C 0.8580(2) 0.60466(17) 0.6495(3) 0.0261(8) Uani 1 1 d . . . . .
C6 C 0.9311(2) 0.61866(17) 0.6118(3) 0.0296(9) Uani 1 1 d . . . . .
H6 H 0.9372 0.6035 0.5387 0.036 Uiso 1 1 calc R U . . .
C7 C 0.9954(2) 0.65324(17) 0.6741(3) 0.0286(9) Uani 1 1 d . . . . .
C8 C 0.9850(2) 0.67424(18) 0.7813(3) 0.0299(9) Uani 1 1 d . . . . .
H8 H 1.0283 0.6967 0.8278 0.036 Uiso 1 1 calc R U . . .
C9 C 0.9133(2) 0.66316(17) 0.8214(3) 0.0248(8) Uani 1 1 d . . . . .
C10 C 0.7904(2) 0.56307(18) 0.5776(3) 0.0269(8) Uani 1 1 d . . . . .
C11 C 0.7143(2) 0.60637(19) 0.5500(3) 0.0349(9) Uani 1 1 d . . . . .
H11A H 0.6989 0.6240 0.6198 0.052 Uiso 1 1 calc R U . . .
H11B H 0.6700 0.5786 0.5104 0.052 Uiso 1 1 calc R U . . .
H11C H 0.7251 0.6445 0.5020 0.052 Uiso 1 1 calc R U . . .
C12 C 0.7733(2) 0.49871(19) 0.6423(3) 0.0397(10) Uani 1 1 d . . . . .
H12A H 0.7554 0.5116 0.7130 0.060 Uiso 1 1 calc R U . . .
H12B H 0.8230 0.4715 0.6585 0.060 Uiso 1 1 calc R U . . .
H12C H 0.7307 0.4720 0.5966 0.060 Uiso 1 1 calc R U . . .
C13 C 0.8145(2) 0.54001(19) 0.4667(3) 0.0374(10) Uani 1 1 d . . . . .
H13A H 0.7694 0.5150 0.4229 0.056 Uiso 1 1 calc R U . . .
H13B H 0.8622 0.5103 0.4819 0.056 Uiso 1 1 calc R U . . .
H13C H 0.8276 0.5798 0.4240 0.056 Uiso 1 1 calc R U . . .
C14 C 1.0757(2) 0.66438(19) 0.6314(3) 0.0339(9) Uani 1 1 d . . . . .
C15 C 1.1044(2) 0.7384(2) 0.6508(3) 0.0434(11) Uani 1 1 d . . . . .
H15A H 1.0643 0.7691 0.6088 0.065 Uiso 1 1 calc R U . . .
H15B H 1.1567 0.7442 0.6246 0.065 Uiso 1 1 calc R U . . .
H15C H 1.1106 0.7491 0.7312 0.065 Uiso 1 1 calc R U . . .
C16 C 1.1397(2) 0.6177(2) 0.6981(3) 0.0405(10) Uani 1 1 d . . . . .
H16A H 1.1470 0.6301 0.7780 0.061 Uiso 1 1 calc R U . . .
H16B H 1.1913 0.6229 0.6700 0.061 Uiso 1 1 calc R U . . .
H16C H 1.1216 0.5703 0.6891 0.061 Uiso 1 1 calc R U . . .
C17 C 1.0713(2) 0.6482(2) 0.5055(3) 0.0441(11) Uani 1 1 d . . . . .
H17A H 1.0577 0.6001 0.4923 0.066 Uiso 1 1 calc R U . . .
H17B H 1.1240 0.6576 0.4825 0.066 Uiso 1 1 calc R U . . .
H17C H 1.0295 0.6765 0.4615 0.066 Uiso 1 1 calc R U . . .
C18 C 0.9018(2) 0.68511(17) 0.9365(3) 0.0263(8) Uani 1 1 d . . . . .
H18A H 0.9529 0.7053 0.9756 0.032 Uiso 1 1 calc R U . . .
H18B H 0.8592 0.7205 0.9303 0.032 Uiso 1 1 calc R U . . .
C19 C 0.9415(2) 0.57312(19) 1.0163(3) 0.0341(9) Uani 1 1 d . . . . .
H19A H 0.9951 0.5929 1.0094 0.041 Uiso 1 1 calc R U . . .
H19B H 0.9280 0.5382 0.9570 0.041 Uiso 1 1 calc R U . . .
C20 C 0.9436(2) 0.5417(2) 1.1316(3) 0.0402(10) Uani 1 1 d . . . . .
H20A H 0.9986 0.5454 1.1761 0.048 Uiso 1 1 calc R U . . .
H20B H 0.9283 0.4930 1.1248 0.048 Uiso 1 1 calc R U . . .
C21 C 0.8827(2) 0.58130(18) 1.1873(3) 0.0334(9) Uani 1 1 d . . . . .
H21A H 0.9037 0.5895 1.2678 0.040 Uiso 1 1 calc R U . . .
H21B H 0.8305 0.5565 1.1812 0.040 Uiso 1 1 calc R U . . .
C22 C 0.8722(2) 0.64826(18) 1.1221(3) 0.0292(9) Uani 1 1 d . . . . .
H22 H 0.9198 0.6779 1.1499 0.035 Uiso 1 1 calc R U . . .
C23 C 0.7962(2) 0.68975(18) 1.1216(3) 0.0263(8) Uani 1 1 d . . . . .
H23 H 0.8054 0.7357 1.0902 0.032 Uiso 1 1 calc R U . . .
C24 C 0.7690(2) 0.69976(19) 1.2375(3) 0.0328(9) Uani 1 1 d . . . . .
H24A H 0.8061 0.6755 1.2969 0.039 Uiso 1 1 calc R U . . .
H24B H 0.7688 0.7486 1.2571 0.039 Uiso 1 1 calc R U . . .
C25 C 0.6829(2) 0.6702(2) 1.2260(3) 0.0364(10) Uani 1 1 d . . . . .
H25A H 0.6753 0.6449 1.2947 0.044 Uiso 1 1 calc R U . . .
H25B H 0.6416 0.7066 1.2122 0.044 Uiso 1 1 calc R U . . .
C26 C 0.6772(2) 0.62282(18) 1.1258(3) 0.0276(9) Uani 1 1 d . . . . .
H26A H 0.7004 0.5777 1.1491 0.033 Uiso 1 1 calc R U . . .
H26B H 0.6200 0.6168 1.0903 0.033 Uiso 1 1 calc R U . . .
C27 C 0.6765(2) 0.71297(17) 0.9835(3) 0.0260(8) Uani 1 1 d . . . . .
H27A H 0.6696 0.7497 1.0375 0.031 Uiso 1 1 calc R U . . .
H27B H 0.7076 0.7320 0.9272 0.031 Uiso 1 1 calc R U . . .
C28 C 0.5942(2) 0.69193(17) 0.9244(3) 0.0251(8) Uani 1 1 d . . . . .
C29 C 0.5307(2) 0.73647(18) 0.9262(3) 0.0301(9) Uani 1 1 d . . . . .
H29 H 0.5401 0.7776 0.9675 0.036 Uiso 1 1 calc R U . . .
C30 C 0.4531(2) 0.72278(18) 0.8692(3) 0.0291(9) Uani 1 1 d . . . . .
C31 C 0.4440(2) 0.66140(18) 0.8128(3) 0.0280(9) Uani 1 1 d . . . . .
H31 H 0.3918 0.6510 0.7724 0.034 Uiso 1 1 calc R U . . .
C32 C 0.5051(2) 0.61355(17) 0.8105(3) 0.0238(8) Uani 1 1 d . . . . .
C33 C 0.5839(2) 0.62978(17) 0.8675(3) 0.0230(8) Uani 1 1 d . . . . .
C34 C 0.4886(2) 0.54566(17) 0.7477(3) 0.0282(9) Uani 1 1 d . . . . .
C35 C 0.4005(2) 0.5390(2) 0.6898(3) 0.0379(10) Uani 1 1 d . . . . .
H35A H 0.3642 0.5425 0.7461 0.057 Uiso 1 1 calc R U . . .
H35B H 0.3928 0.4947 0.6521 0.057 Uiso 1 1 calc R U . . .
H35C H 0.3880 0.5754 0.6342 0.057 Uiso 1 1 calc R U . . .
C36 C 0.5056(2) 0.48655(17) 0.8308(3) 0.0337(9) Uani 1 1 d . . . . .
H36A H 0.5625 0.4880 0.8668 0.051 Uiso 1 1 calc R U . . .
H36B H 0.4948 0.4434 0.7905 0.051 Uiso 1 1 calc R U . . .
H36C H 0.4704 0.4904 0.8883 0.051 Uiso 1 1 calc R U . . .
C37 C 0.5429(2) 0.53915(19) 0.6567(3) 0.0382(10) Uani 1 1 d . . . . .
H37A H 0.5305 0.5760 0.6019 0.057 Uiso 1 1 calc R U . . .
H37B H 0.5330 0.4952 0.6185 0.057 Uiso 1 1 calc R U . . .
H37C H 0.6000 0.5420 0.6916 0.057 Uiso 1 1 calc R U . . .
C38 C 0.3856(2) 0.77423(19) 0.8725(3) 0.0347(9) Uani 1 1 d . . . . .
C39 C 0.4081(3) 0.8418(2) 0.8224(4) 0.0629(14) Uani 1 1 d . . . . .
H39A H 0.4595 0.8584 0.8646 0.094 Uiso 1 1 calc R U . . .
H39B H 0.3652 0.8753 0.8271 0.094 Uiso 1 1 calc R U . . .
H39C H 0.4140 0.8351 0.7435 0.094 Uiso 1 1 calc R U . . .
C40 C 0.3724(3) 0.7857(2) 0.9936(3) 0.0586(13) Uani 1 1 d . . . . .
H40A H 0.3569 0.7427 1.0255 0.088 Uiso 1 1 calc R U . . .
H40B H 0.3290 0.8192 0.9948 0.088 Uiso 1 1 calc R U . . .
H40C H 0.4226 0.8026 1.0382 0.088 Uiso 1 1 calc R U . . .
C41 C 0.3055(2) 0.7510(2) 0.8052(3) 0.0468(11) Uani 1 1 d . . . . .
H41A H 0.3125 0.7427 0.7271 0.070 Uiso 1 1 calc R U . . .
H41B H 0.2644 0.7864 0.8073 0.070 Uiso 1 1 calc R U . . .
H41C H 0.2879 0.7090 0.8379 0.070 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Al1 O1 1.718(2) . ?
Al1 O2 1.759(2) . ?
Al1 O3 1.796(2) . ?
Al1 N2 2.022(3) . ?
Al1 N1 2.253(3) . ?
O1 C1 1.403(4) . ?
N1 C18 1.489(4) . ?
N1 C19 1.491(4) . ?
N1 C22 1.498(4) . ?
C1 C3 1.506(5) . ?
C1 C2 1.508(5) . ?
O2 C4 1.346(4) . ?
N2 C27 1.503(4) . ?
N2 C26 1.504(4) . ?
N2 C23 1.520(4) . ?
O3 C33 1.340(4) . ?
C4 C5 1.400(4) . ?
C4 C9 1.406(5) . ?
C5 C6 1.394(5) . ?
C5 C10 1.543(5) . ?
C6 C7 1.386(5) . ?
C7 C8 1.392(4) . ?
C7 C14 1.526(5) . ?
C8 C9 1.375(4) . ?
C9 C18 1.493(4) . ?
C10 C11 1.520(5) . ?
C10 C13 1.524(4) . ?
C10 C12 1.536(5) . ?
C14 C16 1.535(5) . ?
C14 C15 1.539(5) . ?
C14 C17 1.540(5) . ?
C19 C20 1.515(5) . ?
C20 C21 1.519(5) . ?
C21 C22 1.529(5) . ?
C22 C23 1.507(5) . ?
C23 C24 1.547(4) . ?
C24 C25 1.536(5) . ?
C25 C26 1.514(4) . ?
C27 C28 1.502(4) . ?
C28 C29 1.377(4) . ?
C28 C33 1.398(4) . ?
C29 C30 1.392(5) . ?
C30 C31 1.381(5) . ?
C30 C38 1.519(5) . ?
C31 C32 1.390(5) . ?
C32 C33 1.420(4) . ?
C32 C34 1.537(5) . ?
C34 C35 1.530(5) . ?
C34 C36 1.531(5) . ?
C34 C37 1.533(5) . ?
C38 C41 1.520(5) . ?
C38 C40 1.525(5) . ?
C38 C39 1.531(5) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 Al1 O2 119.41(12) . . ?
O1 Al1 O3 103.46(12) . . ?
O2 Al1 O3 94.31(11) . . ?
O1 Al1 N2 115.09(12) . . ?
O2 Al1 N2 122.91(12) . . ?
O3 Al1 N2 88.53(11) . . ?
O1 Al1 N1 88.22(11) . . ?
O2 Al1 N1 86.42(10) . . ?
O3 Al1 N1 165.99(11) . . ?
N2 Al1 N1 79.41(11) . . ?
C1 O1 Al1 129.5(2) . . ?
C18 N1 C19 110.7(3) . . ?
C18 N1 C22 111.8(3) . . ?
C19 N1 C22 104.9(2) . . ?
C18 N1 Al1 107.71(19) . . ?
C19 N1 Al1 115.2(2) . . ?
C22 N1 Al1 106.6(2) . . ?
O1 C1 C3 108.7(3) . . ?
O1 C1 C2 109.6(3) . . ?
C3 C1 C2 111.9(3) . . ?
C4 O2 Al1 134.4(2) . . ?
C27 N2 C26 110.1(2) . . ?
C27 N2 C23 107.1(2) . . ?
C26 N2 C23 104.4(2) . . ?
C27 N2 Al1 105.27(18) . . ?
C26 N2 Al1 113.1(2) . . ?
C23 N2 Al1 116.8(2) . . ?
C33 O3 Al1 133.5(2) . . ?
O2 C4 C5 122.5(3) . . ?
O2 C4 C9 118.3(3) . . ?
C5 C4 C9 119.2(3) . . ?
C6 C5 C4 117.6(3) . . ?
C6 C5 C10 121.5(3) . . ?
C4 C5 C10 121.0(3) . . ?
C7 C6 C5 124.2(3) . . ?
C6 C7 C8 116.6(3) . . ?
C6 C7 C14 122.3(3) . . ?
C8 C7 C14 121.0(3) . . ?
C9 C8 C7 121.4(3) . . ?
C8 C9 C4 120.9(3) . . ?
C8 C9 C18 121.8(3) . . ?
C4 C9 C18 117.3(3) . . ?
C11 C10 C13 107.6(3) . . ?
C11 C10 C12 110.9(3) . . ?
C13 C10 C12 107.1(3) . . ?
C11 C10 C5 109.7(3) . . ?
C13 C10 C5 112.2(3) . . ?
C12 C10 C5 109.3(3) . . ?
C7 C14 C16 108.2(3) . . ?
C7 C14 C15 110.7(3) . . ?
C16 C14 C15 108.2(3) . . ?
C7 C14 C17 113.3(3) . . ?
C16 C14 C17 108.2(3) . . ?
C15 C14 C17 108.1(3) . . ?
N1 C18 C9 111.8(3) . . ?
N1 C19 C20 107.1(3) . . ?
C19 C20 C21 106.0(3) . . ?
C20 C21 C22 104.2(3) . . ?
N1 C22 C23 109.1(3) . . ?
N1 C22 C21 103.3(3) . . ?
C23 C22 C21 119.8(3) . . ?
C22 C23 N2 110.2(3) . . ?
C22 C23 C24 115.6(3) . . ?
N2 C23 C24 106.6(3) . . ?
C25 C24 C23 105.9(3) . . ?
C26 C25 C24 104.2(3) . . ?
N2 C26 C25 105.4(3) . . ?
C28 C27 N2 114.6(3) . . ?
C29 C28 C33 121.9(3) . . ?
C29 C28 C27 117.7(3) . . ?
C33 C28 C27 120.3(3) . . ?
C28 C29 C30 121.8(3) . . ?
C31 C30 C29 115.6(3) . . ?
C31 C30 C38 124.8(3) . . ?
C29 C30 C38 119.6(3) . . ?
C30 C31 C32 125.3(3) . . ?
C31 C32 C33 117.6(3) . . ?
C31 C32 C34 121.5(3) . . ?
C33 C32 C34 120.8(3) . . ?
O3 C33 C28 119.9(3) . . ?
O3 C33 C32 122.3(3) . . ?
C28 C33 C32 117.7(3) . . ?
C35 C34 C36 107.3(3) . . ?
C35 C34 C37 107.6(3) . . ?
C36 C34 C37 109.5(3) . . ?
C35 C34 C32 112.5(3) . . ?
C36 C34 C32 109.7(3) . . ?
C37 C34 C32 110.1(3) . . ?
C30 C38 C41 112.3(3) . . ?
C30 C38 C40 110.1(3) . . ?
C41 C38 C40 107.8(3) . . ?
C30 C38 C39 109.8(3) . . ?
C41 C38 C39 107.5(3) . . ?
C40 C38 C39 109.3(3) . . ?
 
_refine_diff_density_max    0.419
_refine_diff_density_min   -0.382
_refine_diff_density_rms    0.067

#===END


data_Hf(3)(OiPr)2

# start Validation Reply Form
_vrf_PLAT413_Hf(3)(OiPr)2
;
PROBLEM: Short Inter XH3 .. XHn     H5B    ..  H31C    ..       1.88 Ang.  
RESPONSE: This is a reflection of the disorder of the isopropyl group
C4-C6.  It is likely that the methyl group C31 could twist in response
to the disorder but it was not possible to model this from the data in 
the presence of heavy atoms.
;
# end Validation Reply Form
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C32 H48 Hf N2 O4' 
_chemical_formula_weight          703.21

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'
 'Hf'  'Hf'  -6.1794   4.9776
 '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'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    14.04840(10)
_cell_length_b                    13.41180(10)
_cell_length_c                    16.83440(10)
_cell_angle_alpha                 90
_cell_angle_beta                  101.4040(10)
_cell_angle_gamma                 90
_cell_volume                      3109.22(4)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used   19809
_cell_measurement_theta_min     4.2390
_cell_measurement_theta_max     71.8630 
_exptl_crystal_description                'block'
_exptl_crystal_colour                     'clear light colourless'
_exptl_crystal_size_max                            0.2000
_exptl_crystal_size_mid                            0.1000
_exptl_crystal_size_min                            0.0500
_exptl_crystal_density_diffrn     1.502          
_exptl_crystal_F_000              1432
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_absorpt_coefficient_mu     6.493
_shelx_estimated_absorpt_T_min    0.027
_shelx_estimated_absorpt_T_max    0.737
_exptl_absorpt_correction_T_min                   0.51878
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_correction_type            'multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature       150(2)
_diffrn_ambient_environment 'N~2~'
_diffrn_source 'sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe 'x-ray'
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_radiation_monochromator 'mirror'
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector 'CCD plate'
_diffrn_detector_type 'EosS2'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number             41339
_diffrn_reflns_av_unetI/netI      0.0359
_diffrn_reflns_av_R_equivalents   0.0675
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          4.248
_diffrn_reflns_theta_max          71.968
_diffrn_reflns_theta_full         67.684
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              6117
_reflns_number_gt                 5568
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
_diffrn_measurement_method 'ω scans'
 
_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.
;
 
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution     SHELXS
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           
;
Two isopropyl groups are disordered over two positions (C1 C2 C3
and the second position C1A C2A C3A; C4 C5 C6 and the second 
position C4A C5A C6A).  The occupancies were allowed to freely
refine and then fixed to the converged values of 50:50 for C1-C3
and 55:45 for C4-C6.  There is significant thermal movement of
the two related groups C4-C6 and C4A-C6A.  This resulted in
significantly elongated adps for these atoms.  Due to the close
proximity of atoms C4 and C4A, the adps were constrained to take
the same value.  The best model obtained also had the adps of
atoms C5 and C6 to be constrained to take the same value and 
C5A and C6A to take the same value.  The thermal motion of these
pairs of atoms could be expected to be similar.  The adps are
still significantly elongated but this was not modelled further
as this reflects the increased freedom for these groups to move.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0691P)²+2.4943P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          6117
_refine_ls_number_parameters      402
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0427
_refine_ls_R_factor_gt            0.0394
_refine_ls_wR_factor_ref          0.1081
_refine_ls_wR_factor_gt           0.1042
_refine_ls_goodness_of_fit_ref    1.042
_refine_ls_restrained_S_all       1.042
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
Hf1 Hf 0.27975(2) 0.15585(2) 0.11107(2) 0.03272(9) Uani 1 1 d . . . . .
O1 O 0.2936(3) 0.0256(2) 0.0649(2) 0.0560(9) Uani 1 1 d . . . . .
N1 N 0.2836(2) 0.3126(2) 0.18285(17) 0.0279(6) Uani 1 1 d . . . . .
O2 O 0.1628(2) 0.1262(2) 0.1564(2) 0.0448(7) Uani 1 1 d . . . . .
N2 N 0.3739(2) 0.1215(2) 0.24109(18) 0.0326(6) Uani 1 1 d . . . . .
O3 O 0.2126(2) 0.2412(2) 0.01890(16) 0.0389(6) Uani 1 1 d . . . . .
O4 O 0.41523(18) 0.2056(2) 0.09534(14) 0.0328(5) Uani 1 1 d . . . . .
C7 C 0.1817(3) 0.3344(3) 0.0054(2) 0.0360(8) Uani 1 1 d . . . . .
C8 C 0.1048(3) 0.3546(4) -0.0593(3) 0.0440(10) Uani 1 1 d . . . . .
C9 C 0.0765(3) 0.4528(4) -0.0756(2) 0.0475(11) Uani 1 1 d . . . . .
H9 H 0.0249 0.4662 -0.1200 0.057 Uiso 1 1 calc R U . . .
C10 C 0.1207(3) 0.5320(4) -0.0297(2) 0.0442(10) Uani 1 1 d . . . . .
C11 C 0.1930(3) 0.5098(3) 0.0369(2) 0.0396(8) Uani 1 1 d . . . . .
H11 H 0.2217 0.5627 0.0709 0.047 Uiso 1 1 calc R U . . .
C12 C 0.2250(3) 0.4131(3) 0.0555(2) 0.0340(8) Uani 1 1 d . . . . .
C13 C 0.0548(3) 0.2697(5) -0.1085(3) 0.0557(13) Uani 1 1 d . . . . .
H13A H 0.0203 0.2291 -0.0749 0.084 Uiso 1 1 calc R U . . .
H13B H 0.1032 0.2285 -0.1279 0.084 Uiso 1 1 calc R U . . .
H13C H 0.0083 0.2960 -0.1550 0.084 Uiso 1 1 calc R U . . .
C14 C 0.0894(4) 0.6378(4) -0.0503(3) 0.0587(14) Uani 1 1 d . . . . .
H14A H 0.1170 0.6816 -0.0049 0.088 Uiso 1 1 calc R U . . .
H14B H 0.0184 0.6418 -0.0604 0.088 Uiso 1 1 calc R U . . .
H14C H 0.1125 0.6587 -0.0989 0.088 Uiso 1 1 calc R U . . .
C15 C 0.3062(3) 0.3942(3) 0.1271(2) 0.0326(7) Uani 1 1 d . . . . .
H15A H 0.3201 0.4567 0.1585 0.039 Uiso 1 1 calc R U . . .
H15B H 0.3654 0.3757 0.1070 0.039 Uiso 1 1 calc R U . . .
C16 C 0.1963(3) 0.3428(3) 0.2159(2) 0.0333(8) Uani 1 1 d . . . . .
H16A H 0.1652 0.2836 0.2351 0.040 Uiso 1 1 calc R U . . .
H16B H 0.1482 0.3767 0.1737 0.040 Uiso 1 1 calc R U . . .
C17 C 0.2334(3) 0.4142(3) 0.2869(3) 0.0419(9) Uani 1 1 d . . . . .
H17A H 0.2209 0.4843 0.2698 0.050 Uiso 1 1 calc R U . . .
H17B H 0.2008 0.4004 0.3328 0.050 Uiso 1 1 calc R U . . .
C18 C 0.3432(3) 0.3948(3) 0.3117(2) 0.0359(8) Uani 1 1 d . . . . .
H18A H 0.3605 0.3740 0.3692 0.043 Uiso 1 1 calc R U . . .
H18B H 0.3804 0.4557 0.3044 0.043 Uiso 1 1 calc R U . . .
C19 C 0.3653(3) 0.3102(3) 0.2553(2) 0.0298(7) Uani 1 1 d . . . . .
H19 H 0.4270 0.3268 0.2371 0.036 Uiso 1 1 calc R U . . .
C20 C 0.3781(3) 0.2090(3) 0.2991(2) 0.0318(7) Uani 1 1 d . . . . .
H20 H 0.4447 0.2090 0.3337 0.038 Uiso 1 1 calc R U . . .
C21 C 0.3079(3) 0.1799(3) 0.3542(2) 0.0414(9) Uani 1 1 d . . . . .
H21A H 0.3230 0.2157 0.4066 0.050 Uiso 1 1 calc R U . . .
H21B H 0.2396 0.1934 0.3278 0.050 Uiso 1 1 calc R U . . .
C22 C 0.3267(4) 0.0688(3) 0.3653(3) 0.0459(10) Uani 1 1 d . . . . .
H22A H 0.3894 0.0557 0.4025 0.055 Uiso 1 1 calc R U . . .
H22B H 0.2739 0.0354 0.3863 0.055 Uiso 1 1 calc R U . . .
C23 C 0.3291(3) 0.0356(3) 0.2800(3) 0.0430(9) Uani 1 1 d . . . . .
H23A H 0.2626 0.0216 0.2496 0.052 Uiso 1 1 calc R U . . .
H23B H 0.3688 -0.0255 0.2806 0.052 Uiso 1 1 calc R U . . .
C24 C 0.4743(3) 0.0880(3) 0.2346(2) 0.0365(8) Uani 1 1 d . . . . .
H24A H 0.5072 0.0627 0.2883 0.044 Uiso 1 1 calc R U . . .
H24B H 0.4678 0.0312 0.1963 0.044 Uiso 1 1 calc R U . . .
C25 C 0.5388(3) 0.1640(3) 0.2075(2) 0.0333(8) Uani 1 1 d . . . . .
C26 C 0.6334(3) 0.1768(3) 0.2492(2) 0.0408(9) Uani 1 1 d . . . . .
H26 H 0.6547 0.1421 0.2987 0.049 Uiso 1 1 calc R U . . .
C27 C 0.6980(3) 0.2391(4) 0.2204(3) 0.0466(10) Uani 1 1 d . . . . .
C28 C 0.6644(3) 0.2895(3) 0.1491(2) 0.0394(8) Uani 1 1 d . . . . .
H28 H 0.7082 0.3316 0.1285 0.047 Uiso 1 1 calc R U . . .
C29 C 0.5695(3) 0.2817(3) 0.1058(2) 0.0349(8) Uani 1 1 d . . . . .
C30 C 0.5059(3) 0.2169(3) 0.1350(2) 0.0307(7) Uani 1 1 d . . . . .
C31 C 0.8017(4) 0.2496(6) 0.2655(3) 0.0695(16) Uani 1 1 d . . . . .
H31A H 0.8446 0.2117 0.2374 0.104 Uiso 1 1 calc R U . . .
H31B H 0.8074 0.2240 0.3207 0.104 Uiso 1 1 calc R U . . .
H31C H 0.8204 0.3202 0.2676 0.104 Uiso 1 1 calc R U . . .
C32 C 0.5355(3) 0.3371(3) 0.0283(3) 0.0416(9) Uani 1 1 d . . . . .
H32A H 0.5910 0.3697 0.0118 0.062 Uiso 1 1 calc R U . . .
H32B H 0.4879 0.3877 0.0363 0.062 Uiso 1 1 calc R U . . .
H32C H 0.5053 0.2904 -0.0140 0.062 Uiso 1 1 calc R U . . .
C1 C 0.3187(6) -0.0482(6) 0.0119(5) 0.0358(17) Uani 0.5 1 d . . P A 1
H1 H 0.2832 -0.0342 -0.0446 0.043 Uiso 0.5 1 calc R U P A 1
C2 C 0.4237(8) -0.0430(8) 0.0143(6) 0.055(2) Uani 0.5 1 d . . P A 1
H2A H 0.4431 0.0268 0.0111 0.083 Uiso 0.5 1 calc R U P A 1
H2B H 0.4392 -0.0800 -0.0317 0.083 Uiso 0.5 1 calc R U P A 1
H2C H 0.4587 -0.0723 0.0650 0.083 Uiso 0.5 1 calc R U P A 1
C3 C 0.2822(12) -0.1428(10) 0.0401(10) 0.077(4) Uani 0.5 1 d . . P A 1
H3A H 0.3071 -0.1505 0.0984 0.116 Uiso 0.5 1 calc R U P A 1
H3B H 0.3043 -0.1988 0.0110 0.116 Uiso 0.5 1 calc R U P A 1
H3C H 0.2111 -0.1417 0.0295 0.116 Uiso 0.5 1 calc R U P A 1
C1A C 0.2823(9) -0.0746(8) 0.0476(6) 0.054(2) Uani 0.5 1 d . . P A 2
H1A H 0.2237 -0.0962 0.0685 0.065 Uiso 0.5 1 calc R U P A 2
C2A C 0.3628(11) -0.1419(9) 0.0862(7) 0.067(3) Uani 0.5 1 d . . P A 2
H2A1 H 0.3764 -0.1315 0.1450 0.101 Uiso 0.5 1 calc R U P A 2
H2A2 H 0.4212 -0.1270 0.0648 0.101 Uiso 0.5 1 calc R U P A 2
H2A3 H 0.3438 -0.2114 0.0743 0.101 Uiso 0.5 1 calc R U P A 2
C3A C 0.2556(11) -0.0814(8) -0.0408(6) 0.072(4) Uani 0.5 1 d . . P A 2
H3A1 H 0.2073 -0.0301 -0.0613 0.109 Uiso 0.5 1 calc R U P A 2
H3A2 H 0.2282 -0.1475 -0.0562 0.109 Uiso 0.5 1 calc R U P A 2
H3A3 H 0.3135 -0.0713 -0.0642 0.109 Uiso 0.5 1 calc R U P A 2
C4 C 0.0806(8) 0.0934(9) 0.1816(7) 0.069(2) Uani 0.55 1 d . . P B 3
H4 H 0.0889 0.1109 0.2403 0.083 Uiso 0.55 1 calc R U P B 3
C5 C 0.0701(11) -0.0212(11) 0.1758(17) 0.155(8) Uani 0.55 1 d . . P B 3
H5A H 0.0089 -0.0412 0.1908 0.232 Uiso 0.55 1 calc R U P B 3
H5B H 0.1246 -0.0526 0.2127 0.232 Uiso 0.55 1 calc R U P B 3
H5C H 0.0701 -0.0426 0.1201 0.232 Uiso 0.55 1 calc R U P B 3
C6 C -0.0026(11) 0.1415(11) 0.1422(18) 0.155(8) Uani 0.55 1 d . . P B 3
H6A H 0.0039 0.2134 0.1525 0.232 Uiso 0.55 1 calc R U P B 3
H6B H -0.0588 0.1162 0.1623 0.232 Uiso 0.55 1 calc R U P B 3
H6C H -0.0117 0.1292 0.0838 0.232 Uiso 0.55 1 calc R U P B 3
C4A C 0.0781(9) 0.0675(12) 0.1332(9) 0.069(2) Uani 0.45 1 d . . P B 4
H4A H 0.1100 0.0027 0.1251 0.083 Uiso 0.45 1 calc R U P B 4
C5A C 0.0189(11) 0.0751(18) 0.0583(9) 0.106(5) Uani 0.45 1 d . . P B 4
H5A1 H -0.0383 0.0325 0.0562 0.160 Uiso 0.45 1 calc R U P B 4
H5A2 H 0.0544 0.0537 0.0167 0.160 Uiso 0.45 1 calc R U P B 4
H5A3 H -0.0020 0.1445 0.0484 0.160 Uiso 0.45 1 calc R U P B 4
C6A C 0.0405(12) 0.0412(19) 0.2021(10) 0.106(5) Uani 0.45 1 d . . P B 4
H6A1 H -0.0066 0.0917 0.2114 0.160 Uiso 0.45 1 calc R U P B 4
H6A2 H 0.0936 0.0376 0.2495 0.160 Uiso 0.45 1 calc R U P B 4
H6A3 H 0.0084 -0.0238 0.1932 0.160 Uiso 0.45 1 calc R U P B 4
 
 
_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
Hf1 O1 1.938(3) . ?
Hf1 O2 1.984(3) . ?
Hf1 O3 2.007(3) . ?
Hf1 O4 2.083(3) . ?
Hf1 N2 2.368(3) . ?
Hf1 N1 2.420(3) . ?
O1 C1A 1.377(11) . ?
O1 C1 1.423(7) . ?
N1 C16 1.499(5) . ?
N1 C19 1.501(4) . ?
N1 C15 1.516(5) . ?
O2 C4 1.379(10) . ?
O2 C4A 1.416(12) . ?
N2 C24 1.504(5) . ?
N2 C20 1.520(4) . ?
N2 C23 1.521(5) . ?
O3 C7 1.328(5) . ?
O4 C30 1.325(4) . ?
C7 C8 1.401(6) . ?
C7 C12 1.411(6) . ?
C8 C9 1.387(7) . ?
C8 C13 1.499(6) . ?
C9 C10 1.387(7) . ?
C10 C11 1.388(6) . ?
C10 C14 1.506(7) . ?
C11 C12 1.388(6) . ?
C12 C15 1.508(5) . ?
C16 C17 1.540(5) . ?
C17 C18 1.538(6) . ?
C18 C19 1.549(5) . ?
C19 C20 1.538(5) . ?
C20 C21 1.533(5) . ?
C21 C22 1.518(6) . ?
C22 C23 1.511(6) . ?
C24 C25 1.494(6) . ?
C25 C26 1.386(6) . ?
C25 C30 1.408(5) . ?
C26 C27 1.390(7) . ?
C27 C28 1.377(7) . ?
C27 C31 1.511(6) . ?
C28 C29 1.391(6) . ?
C29 C30 1.403(5) . ?
C29 C32 1.496(6) . ?
C1 C2 1.469(13) . ?
C1 C3 1.481(15) . ?
C1A C3A 1.464(13) . ?
C1A C2A 1.492(16) . ?
C4 C6 1.38(2) . ?
C4 C5 1.545(19) . ?
C4A C5A 1.37(2) . ?
C4A C6A 1.41(2) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 Hf1 O2 97.47(14) . . ?
O1 Hf1 O3 105.87(14) . . ?
O2 Hf1 O3 96.51(13) . . ?
O1 Hf1 O4 94.08(13) . . ?
O2 Hf1 O4 163.81(11) . . ?
O3 Hf1 O4 91.18(11) . . ?
O1 Hf1 N2 96.50(14) . . ?
O2 Hf1 N2 87.67(12) . . ?
O3 Hf1 N2 156.44(11) . . ?
O4 Hf1 N2 79.76(10) . . ?
O1 Hf1 N1 171.69(14) . . ?
O2 Hf1 N1 85.44(11) . . ?
O3 Hf1 N1 81.43(10) . . ?
O4 Hf1 N1 81.63(10) . . ?
N2 Hf1 N1 75.78(10) . . ?
C1A O1 Hf1 161.5(6) . . ?
C1 O1 Hf1 159.3(4) . . ?
C16 N1 C19 104.7(3) . . ?
C16 N1 C15 108.8(3) . . ?
C19 N1 C15 107.4(3) . . ?
C16 N1 Hf1 118.7(2) . . ?
C19 N1 Hf1 109.0(2) . . ?
C15 N1 Hf1 107.73(19) . . ?
C4 O2 Hf1 171.9(5) . . ?
C4A O2 Hf1 136.1(6) . . ?
C24 N2 C20 111.1(3) . . ?
C24 N2 C23 106.2(3) . . ?
C20 N2 C23 106.0(3) . . ?
C24 N2 Hf1 110.6(2) . . ?
C20 N2 Hf1 112.8(2) . . ?
C23 N2 Hf1 110.0(2) . . ?
C7 O3 Hf1 139.2(2) . . ?
C30 O4 Hf1 141.6(2) . . ?
O3 C7 C8 119.4(4) . . ?
O3 C7 C12 120.9(4) . . ?
C8 C7 C12 119.7(4) . . ?
C9 C8 C7 119.0(4) . . ?
C9 C8 C13 121.8(4) . . ?
C7 C8 C13 119.2(4) . . ?
C10 C9 C8 122.5(4) . . ?
C9 C10 C11 117.5(4) . . ?
C9 C10 C14 121.0(4) . . ?
C11 C10 C14 121.4(5) . . ?
C10 C11 C12 122.3(4) . . ?
C11 C12 C7 118.8(4) . . ?
C11 C12 C15 119.8(4) . . ?
C7 C12 C15 121.4(4) . . ?
C12 C15 N1 113.4(3) . . ?
N1 C16 C17 106.2(3) . . ?
C18 C17 C16 105.8(3) . . ?
C17 C18 C19 105.6(3) . . ?
N1 C19 C20 114.0(3) . . ?
N1 C19 C18 105.6(3) . . ?
C20 C19 C18 111.8(3) . . ?
N2 C20 C21 104.1(3) . . ?
N2 C20 C19 112.8(3) . . ?
C21 C20 C19 119.1(3) . . ?
C22 C21 C20 102.0(3) . . ?
C23 C22 C21 102.0(3) . . ?
C22 C23 N2 106.0(3) . . ?
C25 C24 N2 116.8(3) . . ?
C26 C25 C30 119.6(4) . . ?
C26 C25 C24 120.6(4) . . ?
C30 C25 C24 119.6(4) . . ?
C25 C26 C27 121.7(4) . . ?
C28 C27 C26 117.7(4) . . ?
C28 C27 C31 121.5(5) . . ?
C26 C27 C31 120.8(5) . . ?
C27 C28 C29 123.2(4) . . ?
C28 C29 C30 118.3(4) . . ?
C28 C29 C32 121.8(4) . . ?
C30 C29 C32 119.8(4) . . ?
O4 C30 C29 120.6(3) . . ?
O4 C30 C25 119.8(4) . . ?
C29 C30 C25 119.6(4) . . ?
O1 C1 C2 108.8(6) . . ?
O1 C1 C3 104.5(7) . . ?
C2 C1 C3 116.2(10) . . ?
O1 C1A C3A 105.8(9) . . ?
O1 C1A C2A 116.9(10) . . ?
C3A C1A C2A 115.2(10) . . ?
O2 C4 C6 112.5(13) . . ?
O2 C4 C5 111.9(11) . . ?
C6 C4 C5 111.9(12) . . ?
C5A C4A C6A 121.1(12) . . ?
C5A C4A O2 122.5(12) . . ?
C6A C4A O2 110.1(11) . . ?
 
_refine_diff_density_max    1.249
_refine_diff_density_min   -0.830
_refine_diff_density_rms    0.109


#===END

data_Hf(2)(OiPr)2
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C32 H48 Hf N2 O4' 
_chemical_formula_weight          703.21

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'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Hf'  'Hf'  -6.1794   4.9776
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       tetragonal
_space_group_IT_number            78
_space_group_name_H-M_alt         'P 43'
_space_group_name_Hall            'P 4cw'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x, z+3/4'
 '-x, -y, z+1/2'
 'y, -x, z+1/4'
 
_cell_length_a                    10.38840(10)
_cell_length_b                    10.38840(10)
_cell_length_c                    28.7320(4)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      3100.72(7)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used   9833
_cell_measurement_theta_min     5.2280
_cell_measurement_theta_max     71.8410
 
_exptl_crystal_description                'prism'
_exptl_crystal_colour                     'clear light colourless'
_exptl_crystal_size_max                            0.1000
_exptl_crystal_size_mid                            0.1000
_exptl_crystal_size_min                            0.0500
_exptl_crystal_density_diffrn     1.506          
_exptl_crystal_F_000              1432
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_absorpt_coefficient_mu     6.511
_shelx_estimated_absorpt_T_min    0.356
_shelx_estimated_absorpt_T_max    0.562
_exptl_absorpt_correction_T_min                   0.48140
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_correction_type            'multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature       150(2)
_diffrn_source 'sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe 'x-ray'
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_radiation_monochromator 'mirror'
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector 'CCD plate'
_diffrn_detector_type 'EosS2'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number             5054
_diffrn_reflns_av_unetI/netI      0.0703
_diffrn_reflns_av_R_equivalents    ?
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -35
_diffrn_reflns_limit_l_max        35
_diffrn_reflns_theta_min          4.526
_diffrn_reflns_theta_max          72.029
_diffrn_reflns_theta_full         67.684
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              5054
_reflns_number_gt                 4977
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.959
_reflns_Friedel_fraction_max      1.000
_reflns_Friedel_fraction_full     1.000
_diffrn_measurement_method 'ω scans'
 
_reflns_special_details
;
 _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.
;
 
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution     SHELXS
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component twin.  The crystal was merohedrally 
twinned about the 010 direction by 22%.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1779P)²+13.3402P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Flack x determined using 1736 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.04(4)
_chemical_absolute_configuration  ad
_refine_ls_number_reflns          5054
_refine_ls_number_parameters      361
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0851
_refine_ls_R_factor_gt            0.0845
_refine_ls_wR_factor_ref          0.2237
_refine_ls_wR_factor_gt           0.2228
_refine_ls_goodness_of_fit_ref    1.065
_refine_ls_restrained_S_all       1.065
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
Hf1 Hf 0.73097(8) 0.15322(9) 0.03327(5) 0.0254(3) Uani 1 1 d . . . . .
O1 O 0.7204(17) 0.0071(19) 0.0748(6) 0.032(4) Uani 1 1 d . . . . .
N1 N 0.9040(16) 0.2406(16) 0.0776(6) 0.018(3) Uani 1 1 d . . . . .
C1 C 0.719(3) -0.096(2) 0.1031(10) 0.036(6) Uani 1 1 d . . . . .
H1 H 0.7804 -0.0793 0.1293 0.044 Uiso 1 1 calc R U . . .
O2 O 0.5841(18) 0.1390(19) -0.0119(7) 0.035(4) Uani 1 1 d . . . . .
N2 N 0.8162(15) 0.3353(16) -0.0076(7) 0.019(3) Uani 1 1 d . . . . .
O3 O 0.6415(17) 0.284(2) 0.0769(6) 0.035(4) Uani 1 1 d . . . . .
C3 C 0.589(3) -0.118(3) 0.1237(13) 0.050(8) Uani 1 1 d . . . . .
H3A H 0.5654 -0.0442 0.1430 0.075 Uiso 1 1 calc R U . . .
H3B H 0.5908 -0.1962 0.1428 0.075 Uiso 1 1 calc R U . . .
H3C H 0.5259 -0.1284 0.0986 0.075 Uiso 1 1 calc R U . . .
O4 O 0.8622(17) 0.0652(16) -0.0102(6) 0.032(4) Uani 1 1 d . . . . .
C4 C 0.455(2) 0.126(3) -0.0183(11) 0.045(7) Uani 1 1 d . . . . .
H4 H 0.4418 0.0682 -0.0456 0.054 Uiso 1 1 calc R U . . .
C5 C 0.400(3) 0.259(3) -0.0313(12) 0.047(7) Uani 1 1 d . . . . .
H5A H 0.4022 0.3157 -0.0040 0.070 Uiso 1 1 calc R U . . .
H5B H 0.3114 0.2496 -0.0421 0.070 Uiso 1 1 calc R U . . .
H5C H 0.4527 0.2974 -0.0562 0.070 Uiso 1 1 calc R U . . .
C7 C 0.658(2) 0.355(2) 0.1143(9) 0.032(5) Uani 1 1 d . . . . .
C8 C 0.767(2) 0.338(2) 0.1408(9) 0.032(5) Uani 1 1 d . . . . .
C9 C 0.784(2) 0.418(2) 0.1801(8) 0.033(5) Uani 1 1 d . . . . .
H9 H 0.8605 0.4106 0.1980 0.040 Uiso 1 1 calc R U . . .
C10 C 0.693(3) 0.507(3) 0.1930(10) 0.040(6) Uani 1 1 d . . . . .
C11 C 0.585(3) 0.524(3) 0.1643(11) 0.043(6) Uani 1 1 d . . . . .
H11 H 0.5245 0.5887 0.1719 0.051 Uiso 1 1 calc R U . . .
C12 C 0.564(2) 0.450(3) 0.1264(9) 0.032(5) Uani 1 1 d . . . . .
C13 C 0.447(2) 0.464(3) 0.0950(11) 0.043(7) Uani 1 1 d . . . . .
H13A H 0.4754 0.4697 0.0625 0.064 Uiso 1 1 calc R U . . .
H13B H 0.4002 0.5425 0.1034 0.064 Uiso 1 1 calc R U . . .
H13C H 0.3910 0.3892 0.0989 0.064 Uiso 1 1 calc R U . . .
C15 C 0.868(2) 0.242(2) 0.1291(9) 0.029(5) Uani 1 1 d . . . . .
H15A H 0.8380 0.1551 0.1382 0.035 Uiso 1 1 calc R U . . .
H15B H 0.9466 0.2611 0.1476 0.035 Uiso 1 1 calc R U . . .
C16 C 1.028(2) 0.170(2) 0.0742(9) 0.031(5) Uani 1 1 d . . . . .
H16A H 1.0349 0.1279 0.0434 0.037 Uiso 1 1 calc R U . . .
H16B H 1.0324 0.1025 0.0984 0.037 Uiso 1 1 calc R U . . .
C17 C 1.141(2) 0.265(3) 0.0805(10) 0.036(5) Uani 1 1 d . . . . .
H17A H 1.2009 0.2599 0.0538 0.043 Uiso 1 1 calc R U . . .
H17B H 1.1889 0.2456 0.1095 0.043 Uiso 1 1 calc R U . . .
C18 C 1.076(2) 0.398(2) 0.0832(9) 0.028(5) Uani 1 1 d . . . . .
H18A H 1.0719 0.4291 0.1157 0.034 Uiso 1 1 calc R U . . .
H18B H 1.1232 0.4619 0.0641 0.034 Uiso 1 1 calc R U . . .
C19 C 0.941(2) 0.3734(19) 0.0636(10) 0.028(5) Uani 1 1 d . . . . .
H19 H 0.8790 0.4369 0.0771 0.034 Uiso 1 1 calc R U . . .
C20 C 0.942(2) 0.384(2) 0.0114(9) 0.026(5) Uani 1 1 d . . . . .
H20 H 1.0140 0.3316 -0.0016 0.032 Uiso 1 1 calc R U . . .
C21 C 0.956(2) 0.527(2) -0.0049(9) 0.028(5) Uani 1 1 d . . . . .
H21A H 0.9821 0.5826 0.0213 0.033 Uiso 1 1 calc R U . . .
H21B H 1.0204 0.5339 -0.0301 0.033 Uiso 1 1 calc R U . . .
C22 C 0.820(3) 0.565(2) -0.0228(10) 0.038(6) Uani 1 1 d . . . . .
H22A H 0.7914 0.6463 -0.0085 0.045 Uiso 1 1 calc R U . . .
H22B H 0.8205 0.5745 -0.0571 0.045 Uiso 1 1 calc R U . . .
C23 C 0.736(3) 0.455(3) -0.0084(10) 0.033(5) Uani 1 1 d . . . . .
H23A H 0.6638 0.4454 -0.0306 0.039 Uiso 1 1 calc R U . . .
H23B H 0.6996 0.4719 0.0229 0.039 Uiso 1 1 calc R U . . .
C24 C 0.833(2) 0.298(2) -0.0595(9) 0.028(5) Uani 1 1 d . . . . .
H24A H 0.7522 0.2593 -0.0709 0.033 Uiso 1 1 calc R U . . .
H24B H 0.8493 0.3773 -0.0778 0.033 Uiso 1 1 calc R U . . .
C25 C 0.942(2) 0.205(2) -0.0674(9) 0.027(5) Uani 1 1 d . . . . .
C26 C 1.034(2) 0.231(2) -0.1015(9) 0.031(5) Uani 1 1 d . . . . .
H26 H 1.0271 0.3077 -0.1192 0.037 Uiso 1 1 calc R U . . .
C27 C 1.137(2) 0.148(2) -0.1107(9) 0.031(5) Uani 1 1 d . . . . .
C28 C 1.139(2) 0.035(2) -0.0849(10) 0.034(5) Uani 1 1 d . . . . .
H28 H 1.2062 -0.0246 -0.0911 0.041 Uiso 1 1 calc R U . . .
C29 C 1.050(2) 0.002(2) -0.0503(9) 0.031(5) Uani 1 1 d . . . . .
C30 C 0.950(2) 0.093(2) -0.0422(8) 0.023(4) Uani 1 1 d . . . . .
C31 C 1.056(3) -0.115(3) -0.0241(10) 0.041(6) Uani 1 1 d . . . . .
H31A H 1.1181 -0.1742 -0.0388 0.061 Uiso 1 1 calc R U . . .
H31B H 0.9712 -0.1559 -0.0234 0.061 Uiso 1 1 calc R U . . .
H31C H 1.0843 -0.0965 0.0078 0.061 Uiso 1 1 calc R U . . .
C32 C 1.237(3) 0.177(3) -0.1473(10) 0.041(6) Uani 1 1 d . . . . .
H32A H 1.2263 0.1182 -0.1736 0.061 Uiso 1 1 calc R U . . .
H32B H 1.3231 0.1666 -0.1340 0.061 Uiso 1 1 calc R U . . .
H32C H 1.2260 0.2661 -0.1580 0.061 Uiso 1 1 calc R U . . .
C2 C 0.763(4) -0.217(3) 0.0782(13) 0.056(8) Uani 1 1 d . . . . .
H2A H 0.7072 -0.2333 0.0513 0.084 Uiso 1 1 calc R U . . .
H2B H 0.7581 -0.2908 0.0996 0.084 Uiso 1 1 calc R U . . .
H2C H 0.8520 -0.2065 0.0676 0.084 Uiso 1 1 calc R U . . .
C14 C 0.709(4) 0.589(4) 0.2356(12) 0.059(9) Uani 1 1 d . . . . .
H14A H 0.7288 0.5346 0.2624 0.088 Uiso 1 1 calc R U . . .
H14B H 0.6285 0.6362 0.2415 0.088 Uiso 1 1 calc R U . . .
H14C H 0.7788 0.6509 0.2306 0.088 Uiso 1 1 calc R U . . .
C6 C 0.388(3) 0.066(3) 0.0232(13) 0.053(9) Uani 1 1 d . . . . .
H6A H 0.4420 -0.0017 0.0364 0.080 Uiso 1 1 calc R U . . .
H6B H 0.3055 0.0288 0.0131 0.080 Uiso 1 1 calc R U . . .
H6C H 0.3715 0.1321 0.0468 0.080 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Hf1 O1 1.934(18) . ?
Hf1 O2 2.009(17) . ?
Hf1 O4 2.062(17) . ?
Hf1 O3 2.073(17) . ?
Hf1 N1 2.383(16) . ?
Hf1 N2 2.396(16) . ?
O1 C1 1.35(3) . ?
N1 C19 1.49(2) . ?
N1 C16 1.49(3) . ?
N1 C15 1.52(3) . ?
C1 C3 1.49(4) . ?
C1 C2 1.52(4) . ?
O2 C4 1.36(3) . ?
N2 C20 1.50(3) . ?
N2 C23 1.50(3) . ?
N2 C24 1.55(3) . ?
O3 C7 1.31(3) . ?
O4 C30 1.33(3) . ?
C4 C6 1.52(5) . ?
C4 C5 1.54(4) . ?
C7 C8 1.37(4) . ?
C7 C12 1.43(3) . ?
C8 C9 1.42(4) . ?
C8 C15 1.49(3) . ?
C9 C10 1.37(4) . ?
C10 C11 1.40(4) . ?
C10 C14 1.50(4) . ?
C11 C12 1.35(4) . ?
C12 C13 1.52(4) . ?
C16 C17 1.54(3) . ?
C17 C18 1.54(4) . ?
C18 C19 1.53(3) . ?
C19 C20 1.51(3) . ?
C20 C21 1.56(3) . ?
C21 C22 1.55(4) . ?
C22 C23 1.49(4) . ?
C24 C25 1.51(3) . ?
C25 C30 1.38(3) . ?
C25 C26 1.40(3) . ?
C26 C27 1.40(4) . ?
C27 C28 1.39(4) . ?
C27 C32 1.51(3) . ?
C28 C29 1.40(4) . ?
C29 C30 1.42(3) . ?
C29 C31 1.43(4) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 Hf1 O2 107.3(8) . . ?
O1 Hf1 O4 93.6(7) . . ?
O2 Hf1 O4 94.5(7) . . ?
O1 Hf1 O3 96.8(8) . . ?
O2 Hf1 O3 95.7(7) . . ?
O4 Hf1 O3 162.6(7) . . ?
O1 Hf1 N1 90.7(7) . . ?
O2 Hf1 N1 161.2(7) . . ?
O4 Hf1 N1 89.7(7) . . ?
O3 Hf1 N1 76.3(7) . . ?
O1 Hf1 N2 160.6(7) . . ?
O2 Hf1 N2 91.2(7) . . ?
O4 Hf1 N2 79.0(6) . . ?
O3 Hf1 N2 86.8(7) . . ?
N1 Hf1 N2 71.5(6) . . ?
C1 O1 Hf1 177.2(18) . . ?
C19 N1 C16 102.3(17) . . ?
C19 N1 C15 108.5(17) . . ?
C16 N1 C15 106.2(17) . . ?
C19 N1 Hf1 113.8(14) . . ?
C16 N1 Hf1 115.6(13) . . ?
C15 N1 Hf1 109.9(12) . . ?
O1 C1 C3 112(2) . . ?
O1 C1 C2 112(3) . . ?
C3 C1 C2 109(2) . . ?
C4 O2 Hf1 147(2) . . ?
C20 N2 C23 102.0(17) . . ?
C20 N2 C24 109.6(17) . . ?
C23 N2 C24 104.8(17) . . ?
C20 N2 Hf1 114.1(14) . . ?
C23 N2 Hf1 117.2(14) . . ?
C24 N2 Hf1 108.5(12) . . ?
C7 O3 Hf1 143.4(16) . . ?
C30 O4 Hf1 141.2(15) . . ?
O2 C4 C6 113(3) . . ?
O2 C4 C5 108(3) . . ?
C6 C4 C5 113(3) . . ?
O3 C7 C8 119(2) . . ?
O3 C7 C12 119(2) . . ?
C8 C7 C12 121(3) . . ?
C7 C8 C9 118(2) . . ?
C7 C8 C15 123(2) . . ?
C9 C8 C15 119(2) . . ?
C10 C9 C8 122(2) . . ?
C9 C10 C11 118(3) . . ?
C9 C10 C14 122(3) . . ?
C11 C10 C14 120(3) . . ?
C12 C11 C10 122(3) . . ?
C11 C12 C7 118(3) . . ?
C11 C12 C13 124(3) . . ?
C7 C12 C13 118(2) . . ?
C8 C15 N1 113(2) . . ?
N1 C16 C17 110(2) . . ?
C16 C17 C18 104.4(18) . . ?
C19 C18 C17 103.3(17) . . ?
N1 C19 C20 109.7(19) . . ?
N1 C19 C18 107(2) . . ?
C20 C19 C18 111(2) . . ?
N2 C20 C19 110(2) . . ?
N2 C20 C21 107(2) . . ?
C19 C20 C21 111.6(19) . . ?
C22 C21 C20 104.8(18) . . ?
C23 C22 C21 104(2) . . ?
C22 C23 N2 108(2) . . ?
C25 C24 N2 113.0(19) . . ?
C30 C25 C26 119(2) . . ?
C30 C25 C24 121(2) . . ?
C26 C25 C24 120(2) . . ?
C25 C26 C27 123(2) . . ?
C28 C27 C26 116(2) . . ?
C28 C27 C32 122(2) . . ?
C26 C27 C32 122(2) . . ?
C27 C28 C29 125(2) . . ?
C28 C29 C30 116(2) . . ?
C28 C29 C31 123(2) . . ?
C30 C29 C31 121(2) . . ?
O4 C30 C25 120(2) . . ?
O4 C30 C29 118(2) . . ?
C25 C30 C29 121(2) . . ?
 
_refine_diff_density_max    1.917
_refine_diff_density_min   -3.543
_refine_diff_density_rms    0.202

#===END

data_Hf(1)(OiPr)2
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C32 H48 Hf N2 O4' 
_chemical_formula_weight          703.21

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'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Hf'  'Hf'  -6.1794   4.9776
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       tetragonal
_space_group_IT_number            76
_space_group_name_H-M_alt         'P 41'
_space_group_name_Hall            'P 4w'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x, z+1/4'
 '-x, -y, z+1/2'
 'y, -x, z+3/4'
 
_cell_length_a                    10.39461(5)
_cell_length_b                    10.39461(5)
_cell_length_c                    28.7569(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      3107.12(4)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used   31198
_cell_measurement_theta_min     4.5210
_cell_measurement_theta_max     71.0290
 
_exptl_crystal_description                'prism'
_exptl_crystal_colour                     'clear pale colourless'
_exptl_crystal_size_max                            0.3000
_exptl_crystal_size_mid                            0.3000
_exptl_crystal_size_min                            0.2000
_exptl_crystal_density_diffrn     1.503          
_exptl_crystal_F_000              1432
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_absorpt_coefficient_mu     6.497
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_T_min                   0.70414
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_correction_type            'multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature       150(2)
_diffrn_ambient_environment 'air'
_diffrn_source 'sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe 'x-ray'
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_radiation_monochromator 'mirror'
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector 'CCD plate'
_diffrn_detector_type 'EosS2'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number             5873
_diffrn_reflns_av_unetI/netI      0.0454
_diffrn_reflns_av_R_equivalents    ?
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -35
_diffrn_reflns_limit_l_max        35
_diffrn_reflns_theta_min          4.253
_diffrn_reflns_theta_max          71.117
_diffrn_reflns_theta_full         67.684
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              5873
_reflns_number_gt                 5867
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.957
_reflns_Friedel_fraction_max      0.997
_reflns_Friedel_fraction_full     1.000
_diffrn_measurement_method 'ω scans'
 
_reflns_special_details
;
 _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.
;
 
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution     SHELXS
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component twin, twinned about the 100 direction
by 40%.  Atoms O4 N2 C19 C23 C16 showed badly behaved adps when
freely refined.  They were therefore constrained to take 
approximately spherical values using the SHELX command ISOR.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1238P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      difmap
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Flack x determined using 2789 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    -0.009(19)
_chemical_absolute_configuration  ad
_refine_ls_number_reflns          5873
_refine_ls_number_parameters      361
_refine_ls_number_restraints      31
_refine_ls_R_factor_all           0.0539
_refine_ls_R_factor_gt            0.0539
_refine_ls_wR_factor_ref          0.1367
_refine_ls_wR_factor_gt           0.1366
_refine_ls_goodness_of_fit_ref    1.040
_refine_ls_restrained_S_all       1.040
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
Hf1 Hf 0.15356(6) 0.26923(5) 0.39899(3) 0.01912(18) Uani 1 1 d . . . . .
O1 O 0.1401(13) 0.4163(11) 0.4424(4) 0.030(3) Uani 1 1 d . . . . .
O2 O 0.0052(13) 0.2817(12) 0.3579(4) 0.030(2) Uani 1 1 d . . . . .
O3 O 0.0664(9) 0.1377(10) 0.4422(4) 0.022(2) Uani 1 1 d . . . . .
O4 O 0.2832(10) 0.3608(9) 0.3565(4) 0.021(2) Uani 1 1 d . U . . .
N1 N 0.3372(12) 0.1841(10) 0.4401(4) 0.017(2) Uani 1 1 d . . . . .
N2 N 0.2410(10) 0.0952(10) 0.3542(4) 0.013(2) Uani 1 1 d . U . . .
C1 C 0.068(2) 0.6126(18) 0.4081(8) 0.048(5) Uani 1 1 d . . . . .
H1A H 0.1084 0.5809 0.3795 0.071 Uiso 1 1 calc R U . . .
H1B H 0.0824 0.7055 0.4108 0.071 Uiso 1 1 calc R U . . .
H1C H -0.0244 0.5951 0.4072 0.071 Uiso 1 1 calc R U . . .
C2 C 0.1273(18) 0.5449(14) 0.4497(6) 0.033(4) Uani 1 1 d . . . . .
H2 H 0.0683 0.5573 0.4768 0.039 Uiso 1 1 calc R U . . .
C4 C -0.0978(17) 0.2801(17) 0.3288(6) 0.031(3) Uani 1 1 d . . . . .
H4 H -0.0796 0.2184 0.3029 0.037 Uiso 1 1 calc R U . . .
C5 C -0.2165(18) 0.237(2) 0.3532(8) 0.048(5) Uani 1 1 d . . . . .
H5A H -0.2206 0.1432 0.3532 0.072 Uiso 1 1 calc R U . . .
H5B H -0.2921 0.2723 0.3373 0.072 Uiso 1 1 calc R U . . .
H5C H -0.2148 0.2687 0.3854 0.072 Uiso 1 1 calc R U . . .
C6 C -0.116(2) 0.412(2) 0.3084(7) 0.045(5) Uani 1 1 d . . . . .
H6A H -0.1002 0.4767 0.3324 0.068 Uiso 1 1 calc R U . . .
H6B H -0.2036 0.4203 0.2966 0.068 Uiso 1 1 calc R U . . .
H6C H -0.0544 0.4241 0.2828 0.068 Uiso 1 1 calc R U . . .
C7 C 0.0946(13) 0.0510(13) 0.4742(4) 0.018(3) Uani 1 1 d . . . . .
C8 C 0.2062(13) 0.0575(14) 0.4997(5) 0.022(3) Uani 1 1 d . . . . .
C9 C 0.2330(15) -0.0342(14) 0.5337(5) 0.025(3) Uani 1 1 d . . . . .
H9 H 0.3106 -0.0285 0.5510 0.030 Uiso 1 1 calc R U . . .
C10 C 0.1475(17) -0.1337(15) 0.5426(5) 0.028(3) Uani 1 1 d . . . . .
C11 C 0.0344(14) -0.1387(15) 0.5175(5) 0.026(3) Uani 1 1 d . . . . .
H11 H -0.0251 -0.2058 0.5240 0.031 Uiso 1 1 calc R U . . .
C12 C 0.0039(13) -0.0499(13) 0.4833(5) 0.020(3) Uani 1 1 d . . . . .
C13 C -0.1173(17) -0.0535(18) 0.4556(6) 0.033(4) Uani 1 1 d . . . . .
H13A H -0.1661 -0.1311 0.4636 0.049 Uiso 1 1 calc R U . . .
H13B H -0.0964 -0.0546 0.4224 0.049 Uiso 1 1 calc R U . . .
H13C H -0.1691 0.0228 0.4626 0.049 Uiso 1 1 calc R U . . .
C14 C 0.1770(19) -0.2344(17) 0.5789(7) 0.037(4) Uani 1 1 d . . . . .
H14A H 0.2071 -0.3131 0.5635 0.056 Uiso 1 1 calc R U . . .
H14B H 0.0990 -0.2533 0.5967 0.056 Uiso 1 1 calc R U . . .
H14C H 0.2440 -0.2023 0.5998 0.056 Uiso 1 1 calc R U . . .
C15 C 0.2989(14) 0.1685(13) 0.4908(5) 0.019(3) Uani 1 1 d . . . . .
H15A H 0.2584 0.2494 0.5015 0.023 Uiso 1 1 calc R U . . .
H15B H 0.3776 0.1548 0.5095 0.023 Uiso 1 1 calc R U . . .
C16 C 0.4519(16) 0.2646(16) 0.4400(5) 0.025(3) Uani 1 1 d . U . . .
H16A H 0.4413 0.3369 0.4621 0.030 Uiso 1 1 calc R U . . .
H16B H 0.4667 0.3006 0.4086 0.030 Uiso 1 1 calc R U . . .
C17 C 0.5664(14) 0.1803(16) 0.4546(6) 0.029(3) Uani 1 1 d . . . . .
H17A H 0.5786 0.1814 0.4887 0.034 Uiso 1 1 calc R U . . .
H17B H 0.6469 0.2088 0.4393 0.034 Uiso 1 1 calc R U . . .
C18 C 0.5254(15) 0.0458(16) 0.4374(5) 0.025(3) Uani 1 1 d . . . . .
H18A H 0.5810 0.0174 0.4114 0.030 Uiso 1 1 calc R U . . .
H18B H 0.5316 -0.0179 0.4629 0.030 Uiso 1 1 calc R U . . .
C19 C 0.3851(13) 0.0594(14) 0.4210(5) 0.017(3) Uani 1 1 d . U . . .
H19 H 0.3328 -0.0127 0.4341 0.020 Uiso 1 1 calc R U . . .
C20 C 0.3739(14) 0.0593(16) 0.3685(5) 0.020(3) Uani 1 1 d . . . . .
H20 H 0.4370 0.1214 0.3549 0.024 Uiso 1 1 calc R U . . .
C21 C 0.3975(15) -0.0766(16) 0.3483(5) 0.025(3) Uani 1 1 d . . . . .
H21A H 0.4277 -0.0718 0.3157 0.030 Uiso 1 1 calc R U . . .
H21B H 0.4617 -0.1243 0.3670 0.030 Uiso 1 1 calc R U . . .
C22 C 0.2654(19) -0.1404(15) 0.3512(6) 0.031(3) Uani 1 1 d . . . . .
H22A H 0.2618 -0.2014 0.3776 0.037 Uiso 1 1 calc R U . . .
H22B H 0.2456 -0.1874 0.3221 0.037 Uiso 1 1 calc R U . . .
C23 C 0.1699(14) -0.0285(13) 0.3585(5) 0.023(3) Uani 1 1 d . U . . .
H23A H 0.1007 -0.0327 0.3349 0.027 Uiso 1 1 calc R U . . .
H23B H 0.1302 -0.0350 0.3897 0.027 Uiso 1 1 calc R U . . .
C24 C 0.2394(15) 0.1339(14) 0.3035(4) 0.020(2) Uani 1 1 d . . . . .
H24A H 0.1537 0.1698 0.2960 0.024 Uiso 1 1 calc R U . . .
H24B H 0.2520 0.0561 0.2842 0.024 Uiso 1 1 calc R U . . .
C25 C 0.3412(16) 0.2319(15) 0.2909(5) 0.025(3) Uani 1 1 d . . . . .
C26 C 0.4174(17) 0.2156(16) 0.2524(5) 0.030(3) Uani 1 1 d . . . . .
H26 H 0.4081 0.1401 0.2341 0.036 Uiso 1 1 calc R U . . .
C27 C 0.5084(18) 0.3080(16) 0.2395(6) 0.031(3) Uani 1 1 d . . . . .
C28 C 0.5228(16) 0.4162(17) 0.2684(6) 0.032(3) Uani 1 1 d . . . . .
H28 H 0.5867 0.4784 0.2610 0.038 Uiso 1 1 calc R U . . .
C29 C 0.4479(17) 0.4347(16) 0.3068(5) 0.028(3) Uani 1 1 d . . . . .
C30 C 0.3535(14) 0.3420(14) 0.3177(4) 0.020(2) Uani 1 1 d . . . . .
C31 C 0.4631(17) 0.5515(16) 0.3365(7) 0.038(4) Uani 1 1 d . . . . .
H31A H 0.5354 0.6030 0.3251 0.057 Uiso 1 1 calc R U . . .
H31B H 0.4797 0.5254 0.3687 0.057 Uiso 1 1 calc R U . . .
H31C H 0.3841 0.6028 0.3352 0.057 Uiso 1 1 calc R U . . .
C32 C 0.591(3) 0.289(3) 0.1978(8) 0.060(7) Uani 1 1 d . . . . .
H32A H 0.6684 0.3425 0.2006 0.090 Uiso 1 1 calc R U . . .
H32B H 0.5433 0.3138 0.1698 0.090 Uiso 1 1 calc R U . . .
H32C H 0.6160 0.1984 0.1956 0.090 Uiso 1 1 calc R U . . .
C3 C 0.2589(18) 0.6002(19) 0.4630(8) 0.045(5) Uani 1 1 d . . . . .
H3A H 0.2871 0.5626 0.4925 0.068 Uiso 1 1 calc R U . . .
H3B H 0.2522 0.6938 0.4663 0.068 Uiso 1 1 calc R U . . .
H3C H 0.3215 0.5797 0.4386 0.068 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Hf1 O2 1.947(12) . ?
Hf1 O1 1.979(10) . ?
Hf1 O4 2.053(10) . ?
Hf1 O3 2.058(10) . ?
Hf1 N2 2.399(10) . ?
Hf1 N1 2.412(11) . ?
O1 C2 1.360(18) . ?
O2 C4 1.36(2) . ?
O3 C7 1.321(17) . ?
O4 C30 1.348(16) . ?
N1 C16 1.457(18) . ?
N1 C19 1.493(17) . ?
N1 C15 1.520(17) . ?
N2 C23 1.488(17) . ?
N2 C20 1.489(16) . ?
N2 C24 1.512(16) . ?
C1 C2 1.52(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.53(3) . ?
C2 H2 1.0000 . ?
C4 C5 1.49(2) . ?
C4 C6 1.50(2) . ?
C4 H4 1.0000 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.38(2) . ?
C7 C12 1.434(18) . ?
C8 C9 1.39(2) . ?
C8 C15 1.525(19) . ?
C9 C10 1.39(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.38(2) . ?
C10 C14 1.51(2) . ?
C11 C12 1.39(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.49(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.54(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.54(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.538(19) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.515(17) . ?
C19 H19 1.0000 . ?
C20 C21 1.55(2) . ?
C20 H20 1.0000 . ?
C21 C22 1.53(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.54(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.51(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.37(2) . ?
C25 C30 1.39(2) . ?
C26 C27 1.40(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.41(3) . ?
C27 C32 1.49(2) . ?
C28 C29 1.36(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.41(2) . ?
C29 C31 1.49(2) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 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
O2 Hf1 O1 106.0(5) . . ?
O2 Hf1 O4 97.3(5) . . ?
O1 Hf1 O4 93.7(5) . . ?
O2 Hf1 O3 93.5(5) . . ?
O1 Hf1 O3 95.8(5) . . ?
O4 Hf1 O3 163.0(4) . . ?
O2 Hf1 N2 91.4(5) . . ?
O1 Hf1 N2 161.4(5) . . ?
O4 Hf1 N2 77.4(4) . . ?
O3 Hf1 N2 89.4(4) . . ?
O2 Hf1 N1 161.5(5) . . ?
O1 Hf1 N1 91.7(4) . . ?
O4 Hf1 N1 86.7(4) . . ?
O3 Hf1 N1 79.0(4) . . ?
N2 Hf1 N1 71.7(4) . . ?
C2 O1 Hf1 149.7(12) . . ?
C4 O2 Hf1 175.4(12) . . ?
C7 O3 Hf1 140.9(9) . . ?
C30 O4 Hf1 141.3(9) . . ?
C16 N1 C19 103.0(11) . . ?
C16 N1 C15 106.0(10) . . ?
C19 N1 C15 110.3(10) . . ?
C16 N1 Hf1 115.9(9) . . ?
C19 N1 Hf1 113.8(8) . . ?
C15 N1 Hf1 107.6(8) . . ?
C23 N2 C20 102.8(11) . . ?
C23 N2 C24 107.7(10) . . ?
C20 N2 C24 110.0(11) . . ?
C23 N2 Hf1 114.8(8) . . ?
C20 N2 Hf1 113.1(8) . . ?
C24 N2 Hf1 108.2(7) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C1 111.9(15) . . ?
O1 C2 C3 108.7(16) . . ?
C1 C2 C3 112.6(16) . . ?
O1 C2 H2 107.8 . . ?
C1 C2 H2 107.8 . . ?
C3 C2 H2 107.8 . . ?
O2 C4 C5 111.4(15) . . ?
O2 C4 C6 109.0(15) . . ?
C5 C4 C6 110.8(17) . . ?
O2 C4 H4 108.5 . . ?
C5 C4 H4 108.5 . . ?
C6 C4 H4 108.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C7 C8 121.7(13) . . ?
O3 C7 C12 118.7(13) . . ?
C8 C7 C12 119.6(13) . . ?
C7 C8 C9 120.6(14) . . ?
C7 C8 C15 118.7(13) . . ?
C9 C8 C15 120.7(13) . . ?
C10 C9 C8 120.8(14) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C11 C10 C9 118.5(14) . . ?
C11 C10 C14 120.5(17) . . ?
C9 C10 C14 121.0(16) . . ?
C10 C11 C12 122.7(15) . . ?
C10 C11 H11 118.6 . . ?
C12 C11 H11 118.6 . . ?
C11 C12 C7 117.8(13) . . ?
C11 C12 C13 123.7(14) . . ?
C7 C12 C13 118.5(13) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 C8 114.1(12) . . ?
N1 C15 H15A 108.7 . . ?
C8 C15 H15A 108.7 . . ?
N1 C15 H15B 108.7 . . ?
C8 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
N1 C16 C17 107.9(12) . . ?
N1 C16 H16A 110.1 . . ?
C17 C16 H16A 110.1 . . ?
N1 C16 H16B 110.1 . . ?
C17 C16 H16B 110.1 . . ?
H16A C16 H16B 108.4 . . ?
C16 C17 C18 102.4(11) . . ?
C16 C17 H17A 111.3 . . ?
C18 C17 H17A 111.3 . . ?
C16 C17 H17B 111.3 . . ?
C18 C17 H17B 111.3 . . ?
H17A C17 H17B 109.2 . . ?
C19 C18 C17 106.1(12) . . ?
C19 C18 H18A 110.5 . . ?
C17 C18 H18A 110.5 . . ?
C19 C18 H18B 110.5 . . ?
C17 C18 H18B 110.5 . . ?
H18A C18 H18B 108.7 . . ?
N1 C19 C20 109.9(13) . . ?
N1 C19 C18 106.5(12) . . ?
C20 C19 C18 112.2(12) . . ?
N1 C19 H19 109.4 . . ?
C20 C19 H19 109.4 . . ?
C18 C19 H19 109.4 . . ?
N2 C20 C19 110.2(11) . . ?
N2 C20 C21 105.8(12) . . ?
C19 C20 C21 111.3(13) . . ?
N2 C20 H20 109.8 . . ?
C19 C20 H20 109.8 . . ?
C21 C20 H20 109.8 . . ?
C22 C21 C20 103.5(12) . . ?
C22 C21 H21A 111.1 . . ?
C20 C21 H21A 111.1 . . ?
C22 C21 H21B 111.1 . . ?
C20 C21 H21B 111.1 . . ?
H21A C21 H21B 109.0 . . ?
C21 C22 C23 105.0(12) . . ?
C21 C22 H22A 110.7 . . ?
C23 C22 H22A 110.7 . . ?
C21 C22 H22B 110.7 . . ?
C23 C22 H22B 110.7 . . ?
H22A C22 H22B 108.8 . . ?
N2 C23 C22 108.7(12) . . ?
N2 C23 H23A 109.9 . . ?
C22 C23 H23A 109.9 . . ?
N2 C23 H23B 109.9 . . ?
C22 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
N2 C24 C25 113.8(11) . . ?
N2 C24 H24A 108.8 . . ?
C25 C24 H24A 108.8 . . ?
N2 C24 H24B 108.8 . . ?
C25 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
C26 C25 C30 119.8(16) . . ?
C26 C25 C24 121.0(14) . . ?
C30 C25 C24 119.1(13) . . ?
C25 C26 C27 121.3(16) . . ?
C25 C26 H26 119.3 . . ?
C27 C26 H26 119.3 . . ?
C26 C27 C28 117.7(15) . . ?
C26 C27 C32 120.9(19) . . ?
C28 C27 C32 121(2) . . ?
C29 C28 C27 122.0(16) . . ?
C29 C28 H28 119.0 . . ?
C27 C28 H28 119.0 . . ?
C28 C29 C30 118.7(16) . . ?
C28 C29 C31 121.1(16) . . ?
C30 C29 C31 120.2(14) . . ?
O4 C30 C25 122.0(14) . . ?
O4 C30 C29 117.5(13) . . ?
C25 C30 C29 120.4(14) . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C27 C32 H32A 109.5 . . ?
C27 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C27 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 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
Hf1 O1 C2 C1 22(3) . . . . ?
Hf1 O1 C2 C3 -103(3) . . . . ?
Hf1 O3 C7 C8 24(2) . . . . ?
Hf1 O3 C7 C12 -158.0(11) . . . . ?
O3 C7 C8 C9 179.2(13) . . . . ?
C12 C7 C8 C9 1(2) . . . . ?
O3 C7 C8 C15 0(2) . . . . ?
C12 C7 C8 C15 -177.7(12) . . . . ?
C7 C8 C9 C10 0(2) . . . . ?
C15 C8 C9 C10 178.6(13) . . . . ?
C8 C9 C10 C11 -1(2) . . . . ?
C8 C9 C10 C14 179.0(14) . . . . ?
C9 C10 C11 C12 1(2) . . . . ?
C14 C10 C11 C12 -178.8(14) . . . . ?
C10 C11 C12 C7 0(2) . . . . ?
C10 C11 C12 C13 179.8(15) . . . . ?
O3 C7 C12 C11 -179.0(12) . . . . ?
C8 C7 C12 C11 -1(2) . . . . ?
O3 C7 C12 C13 1(2) . . . . ?
C8 C7 C12 C13 179.0(13) . . . . ?
C16 N1 C15 C8 -163.0(12) . . . . ?
C19 N1 C15 C8 -52.1(15) . . . . ?
Hf1 N1 C15 C8 72.5(12) . . . . ?
C7 C8 C15 N1 -53.0(17) . . . . ?
C9 C8 C15 N1 128.2(14) . . . . ?
C19 N1 C16 C17 -38.8(14) . . . . ?
C15 N1 C16 C17 77.1(14) . . . . ?
Hf1 N1 C16 C17 -163.7(9) . . . . ?
N1 C16 C17 C18 29.1(15) . . . . ?
C16 C17 C18 C19 -7.9(15) . . . . ?
C16 N1 C19 C20 -89.1(14) . . . . ?
C15 N1 C19 C20 158.1(12) . . . . ?
Hf1 N1 C19 C20 37.1(14) . . . . ?
C16 N1 C19 C18 32.6(14) . . . . ?
C15 N1 C19 C18 -80.2(14) . . . . ?
Hf1 N1 C19 C18 158.9(9) . . . . ?
C17 C18 C19 N1 -14.9(15) . . . . ?
C17 C18 C19 C20 105.5(15) . . . . ?
C23 N2 C20 C19 -82.4(15) . . . . ?
C24 N2 C20 C19 163.0(13) . . . . ?
Hf1 N2 C20 C19 41.9(16) . . . . ?
C23 N2 C20 C21 38.0(12) . . . . ?
C24 N2 C20 C21 -76.5(14) . . . . ?
Hf1 N2 C20 C21 162.3(8) . . . . ?
N1 C19 C20 N2 -51.9(18) . . . . ?
C18 C19 C20 N2 -170.2(11) . . . . ?
N1 C19 C20 C21 -169.0(11) . . . . ?
C18 C19 C20 C21 72.7(19) . . . . ?
N2 C20 C21 C22 -34.2(14) . . . . ?
C19 C20 C21 C22 85.6(15) . . . . ?
C20 C21 C22 C23 16.3(15) . . . . ?
C20 N2 C23 C22 -27.6(14) . . . . ?
C24 N2 C23 C22 88.6(13) . . . . ?
Hf1 N2 C23 C22 -150.8(10) . . . . ?
C21 C22 C23 N2 6.6(16) . . . . ?
C23 N2 C24 C25 -161.4(11) . . . . ?
C20 N2 C24 C25 -50.1(15) . . . . ?
Hf1 N2 C24 C25 74.0(12) . . . . ?
N2 C24 C25 C26 132.7(13) . . . . ?
N2 C24 C25 C30 -50.0(17) . . . . ?
C30 C25 C26 C27 0(2) . . . . ?
C24 C25 C26 C27 177.6(14) . . . . ?
C25 C26 C27 C28 2(2) . . . . ?
C25 C26 C27 C32 179.6(17) . . . . ?
C26 C27 C28 C29 -3(2) . . . . ?
C32 C27 C28 C29 -179.8(18) . . . . ?
C27 C28 C29 C30 0(2) . . . . ?
C27 C28 C29 C31 -178.7(15) . . . . ?
Hf1 O4 C30 C25 6(2) . . . . ?
Hf1 O4 C30 C29 -169.6(11) . . . . ?
C26 C25 C30 O4 -178.3(13) . . . . ?
C24 C25 C30 O4 4(2) . . . . ?
C26 C25 C30 C29 -3(2) . . . . ?
C24 C25 C30 C29 179.7(13) . . . . ?
C28 C29 C30 O4 178.3(13) . . . . ?
C31 C29 C30 O4 -3(2) . . . . ?
C28 C29 C30 C25 3(2) . . . . ?
C31 C29 C30 C25 -178.4(14) . . . . ?
 
_refine_diff_density_max    0.952
_refine_diff_density_min   -2.539
_refine_diff_density_rms    0.168

#===END

data_Al(3)(OiPr)


# start Validation Reply Form
_vrf_CHEMW03_Al(3)(OiPr)
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: There are 8 pores within the structure containing 
disordered solvent.  This has been attributed to disordered 
hexane molecules and 8 hexane molecules have therefore been
included in the chemical formula
;
# end Validation Reply Form
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C31 H45.67 Al N2 O3'
_chemical_formula_weight          521.34

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'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Al'  'Al'   0.2130   0.2455
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       cubic
_space_group_IT_number            205
_space_group_name_H-M_alt         'P a -3'
_space_group_name_Hall            '-P 2ac 2ab 3'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 'z, x, y'
 'y, z, x'
 '-y+1/2, -z, x+1/2'
 'z+1/2, -x+1/2, -y'                                                                                                                  
 '-y, z+1/2, -x+1/2'
 '-z+1/2, -x, y+1/2'
 '-z, x+1/2, -y+1/2'
 'y+1/2, -z+1/2, -x'
 '-x+1/2, -y, z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 '-z, -x, -y'
 '-y, -z, -x'
 'y-1/2, z, -x-1/2'
 '-z-1/2, x-1/2, y'
 'y, -z-1/2, x-1/2'
 'z-1/2, x, -y-1/2'
 'z, -x-1/2, y-1/2'
 '-y-1/2, z-1/2, x'
 'x-1/2, y, -z-1/2'
 '-x-1/2, y-1/2, z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    26.25610(10)
_cell_length_b                    26.25610(10)
_cell_length_c                    26.25610(10)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      18100.5(2)
_cell_formula_units_Z             24
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used   37620
_cell_measurement_theta_min     3.7700
_cell_measurement_theta_max     71.7970
_exptl_crystal_description        cube
_exptl_crystal_colour             'clear light colourless'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.148          
_exptl_crystal_F_000              6784
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.300
_exptl_crystal_size_mid           0.200
_exptl_crystal_size_min           0.200
_exptl_absorpt_coefficient_mu     0.835
_shelx_estimated_absorpt_T_min    0.788
_shelx_estimated_absorpt_T_max    0.921
_exptl_absorpt_correction_T_min                   0.65300
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_correction_type            'multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      1.54184
_diffrn_radiation_type            CuK\a
_diffrn_source 'sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator 'mirror'
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector 'CCD plate'
_diffrn_detector_type 'EosS2'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_radiation_probe 'x-ray'
_diffrn_reflns_number             148345
_diffrn_reflns_av_unetI/netI      0.0149
_diffrn_reflns_av_R_equivalents   0.0567
_diffrn_reflns_limit_h_min        -32
_diffrn_reflns_limit_h_max        30
_diffrn_reflns_limit_k_min        -32
_diffrn_reflns_limit_k_max        28
_diffrn_reflns_limit_l_min        -30
_diffrn_reflns_limit_l_max        32
_diffrn_reflns_theta_min          4.124
_diffrn_reflns_theta_max          72.068
_diffrn_reflns_theta_full         67.684
_diffrn_measured_fraction_theta_max   0.995
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.995
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.995
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              5942
_reflns_number_gt                 5460
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
_diffrn_measurement_method 'ω scans'
 
_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.
;
 
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution     'SHELXS'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           
;
There are 8 pores contained within the structure.  All attempts 
to model the solvent resulted in chemically unmeaningful 
residues.  SQUEEZE was therefore used to remove the residual
electron density and to estimate the contents of the pores.
The crystals were grown from hexane and the electron count
per pore and volume of each pore are consistent with one
hexane molecule being contained within each pore.  These 8
extra unmodelled hexane molecules were therefore included in
the chemical formula.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0990P)²+4.4224P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          5942
_refine_ls_number_parameters      322
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0633
_refine_ls_R_factor_gt            0.0588
_refine_ls_wR_factor_ref          0.1716
_refine_ls_wR_factor_gt           0.1671
_refine_ls_goodness_of_fit_ref    1.101
_refine_ls_restrained_S_all       1.101
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000

# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.000       277        47 ' '
   2  0.500  0.000  0.000       230        47 ' '
   3  0.500  0.000  0.500       277        47 ' '
   4  0.000  0.000  0.500       230        47 ' '
   5  0.500  0.500  0.000       277        47 ' '
   6  1.000  0.500  0.500       277        47 ' '
   7  1.000  0.500  0.000       230        47 ' '
   8  0.500  0.500  0.500       230        47 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

 
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
Al1 Al 0.26391(2) 0.64431(2) 0.37027(2) 0.04912(18) Uani 1 1 d . . . . .
O1 O 0.24841(6) 0.60044(5) 0.41713(6) 0.0623(4) Uani 1 1 d . . . . .
N1 N 0.24100(6) 0.61758(5) 0.30013(6) 0.0456(3) Uani 1 1 d . . . . .
C1 C 0.27769(13) 0.56077(9) 0.43747(9) 0.0810(8) Uani 1 1 d . . . . .
H1 H 0.2983 0.5455 0.4093 0.097 Uiso 1 1 calc R U . . .
O2 O 0.32795(6) 0.62778(7) 0.35416(6) 0.0730(5) Uani 1 1 d . . . . .
N2 N 0.18553(6) 0.67150(6) 0.37055(6) 0.0461(3) Uani 1 1 d . . . . .
C2 C 0.2414(2) 0.52028(14) 0.45725(18) 0.154(2) Uani 1 1 d . . . . .
H2A H 0.2232 0.5334 0.4871 0.230 Uiso 1 1 calc R U . . .
H2B H 0.2607 0.4898 0.4668 0.230 Uiso 1 1 calc R U . . .
H2C H 0.2168 0.5115 0.4306 0.230 Uiso 1 1 calc R U . . .
O3 O 0.28328(5) 0.70705(5) 0.38576(5) 0.0527(3) Uani 1 1 d . . . . .
C3 C 0.31294(16) 0.57934(15) 0.47692(13) 0.1182(14) Uani 1 1 d . . . . .
H3A H 0.3350 0.6057 0.4625 0.177 Uiso 1 1 calc R U . . .
H3B H 0.3339 0.5510 0.4893 0.177 Uiso 1 1 calc R U . . .
H3C H 0.2934 0.5937 0.5053 0.177 Uiso 1 1 calc R U . . .
C4 C 0.35309(8) 0.61751(7) 0.31173(9) 0.0555(5) Uani 1 1 d . . . . .
C5 C 0.40434(8) 0.60172(7) 0.31436(10) 0.0588(5) Uani 1 1 d . . . . .
C6 C 0.42891(8) 0.58745(8) 0.27026(10) 0.0637(6) Uani 1 1 d . . . . .
H6 H 0.4635 0.5772 0.2723 0.076 Uiso 1 1 calc R U . . .
C7 C 0.40551(9) 0.58744(9) 0.22329(10) 0.0680(6) Uani 1 1 d . . . . .
C8 C 0.35524(9) 0.60454(8) 0.22077(9) 0.0606(5) Uani 1 1 d . . . . .
H8 H 0.3384 0.6053 0.1888 0.073 Uiso 1 1 calc R U . . .
C9 C 0.32937(8) 0.62039(7) 0.26397(8) 0.0516(4) Uani 1 1 d . . . . .
C10 C 0.42918(9) 0.59845(10) 0.36581(11) 0.0761(7) Uani 1 1 d . . . . .
H10A H 0.4117 0.5727 0.3865 0.114 Uiso 1 1 calc R U . . .
H10B H 0.4270 0.6316 0.3828 0.114 Uiso 1 1 calc R U . . .
H10C H 0.4650 0.5889 0.3617 0.114 Uiso 1 1 calc R U . . .
C11 C 0.43323(13) 0.56839(14) 0.17677(13) 0.0967(9) Uani 1 1 d . . . . .
H11A H 0.4424 0.5973 0.1550 0.145 Uiso 1 1 calc R U . . .
H11B H 0.4111 0.5451 0.1578 0.145 Uiso 1 1 calc R U . . .
H11C H 0.4642 0.5504 0.1872 0.145 Uiso 1 1 calc R U . . .
C12 C 0.27596(8) 0.64038(7) 0.26080(7) 0.0503(4) Uani 1 1 d . . . . .
H12A H 0.2622 0.6331 0.2265 0.060 Uiso 1 1 calc R U . . .
H12B H 0.2766 0.6778 0.2652 0.060 Uiso 1 1 calc R U . . .
C13 C 0.24240(8) 0.56040(7) 0.29585(8) 0.0509(4) Uani 1 1 d . . . . .
H13A H 0.2288 0.5443 0.3271 0.061 Uiso 1 1 calc R U . . .
H13B H 0.2777 0.5483 0.2903 0.061 Uiso 1 1 calc R U . . .
C14 C 0.20911(9) 0.54820(8) 0.25032(9) 0.0611(5) Uani 1 1 d . . . . .
H14A H 0.1950 0.5133 0.2530 0.073 Uiso 1 1 calc R U . . .
H14B H 0.2288 0.5509 0.2183 0.073 Uiso 1 1 calc R U . . .
C15 C 0.16662(9) 0.58781(8) 0.25186(9) 0.0602(5) Uani 1 1 d . . . . .
H15A H 0.1351 0.5729 0.2661 0.072 Uiso 1 1 calc R U . . .
H15B H 0.1593 0.6008 0.2172 0.072 Uiso 1 1 calc R U . . .
C16 C 0.18667(7) 0.63089(7) 0.28646(7) 0.0480(4) Uani 1 1 d . . . . .
H16 H 0.1869 0.6633 0.2664 0.058 Uiso 1 1 calc R U . . .
C17 C 0.15566(7) 0.63933(7) 0.33458(8) 0.0515(4) Uani 1 1 d . . . . .
H17 H 0.1244 0.6588 0.3249 0.062 Uiso 1 1 calc R U . . .
C18 C 0.13906(9) 0.59415(8) 0.36723(10) 0.0639(5) Uani 1 1 d . . . . .
H18A H 0.1082 0.5778 0.3530 0.077 Uiso 1 1 calc R U . . .
H18B H 0.1665 0.5684 0.3697 0.077 Uiso 1 1 calc R U . . .
C19 C 0.12808(11) 0.61776(10) 0.41882(11) 0.0785(7) Uani 1 1 d . . . . .
H19A H 0.1388 0.5946 0.4465 0.094 Uiso 1 1 calc R U . . .
H19B H 0.0912 0.6248 0.4226 0.094 Uiso 1 1 calc R U . . .
C20 C 0.15843(9) 0.66715(8) 0.42077(8) 0.0599(5) Uani 1 1 d . . . . .
H20A H 0.1354 0.6966 0.4259 0.072 Uiso 1 1 calc R U . . .
H20B H 0.1833 0.6662 0.4491 0.072 Uiso 1 1 calc R U . . .
C21 C 0.18472(7) 0.72583(7) 0.35325(7) 0.0449(4) Uani 1 1 d . . . . .
H21A H 0.2025 0.7287 0.3201 0.054 Uiso 1 1 calc R U . . .
H21B H 0.1490 0.7369 0.3484 0.054 Uiso 1 1 calc R U . . .
C22 C 0.21007(7) 0.75962(6) 0.39138(6) 0.0433(4) Uani 1 1 d . . . . .
C23 C 0.25944(7) 0.74714(7) 0.40656(7) 0.0459(4) Uani 1 1 d . . . . .
C24 C 0.28443(8) 0.77744(8) 0.44268(7) 0.0519(4) Uani 1 1 d . . . . .
C25 C 0.25911(9) 0.82013(9) 0.46143(7) 0.0582(5) Uani 1 1 d . . . . .
H25 H 0.2761 0.8412 0.4854 0.070 Uiso 1 1 calc R U . . .
C26 C 0.21001(8) 0.83322(8) 0.44656(7) 0.0545(5) Uani 1 1 d . . . . .
C27 C 0.18566(7) 0.80199(7) 0.41148(7) 0.0474(4) Uani 1 1 d . . . . .
H27 H 0.1519 0.8097 0.4011 0.057 Uiso 1 1 calc R U . . .
C28 C 0.18257(12) 0.87889(10) 0.46806(10) 0.0786(7) Uani 1 1 d . . . . .
H28A H 0.2034 0.8944 0.4949 0.118 Uiso 1 1 calc R U . . .
H28B H 0.1498 0.8681 0.4823 0.118 Uiso 1 1 calc R U . . .
H28C H 0.1767 0.9038 0.4409 0.118 Uiso 1 1 calc R U . . .
C29 C 0.33688(9) 0.76282(11) 0.46063(9) 0.0695(6) Uani 1 1 d . . . . .
H29A H 0.3606 0.7638 0.4318 0.104 Uiso 1 1 calc R U . . .
H29B H 0.3360 0.7283 0.4749 0.104 Uiso 1 1 calc R U . . .
H29C H 0.3482 0.7869 0.4869 0.104 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Al1 O1 1.7340(16) . ?
Al1 O3 1.7713(15) . ?
Al1 O2 1.7872(16) . ?
Al1 N1 2.0605(16) . ?
Al1 N2 2.1785(16) . ?
O1 C1 1.400(3) . ?
N1 C12 1.506(3) . ?
N1 C13 1.506(2) . ?
N1 C16 1.512(2) . ?
C1 C3 1.472(4) . ?
C1 C2 1.520(6) . ?
C1 H1 1.0000 . ?
O2 C4 1.323(3) . ?
N2 C17 1.490(2) . ?
N2 C21 1.497(2) . ?
N2 C20 1.503(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O3 C23 1.341(2) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C9 1.402(3) . ?
C4 C5 1.410(3) . ?
C5 C6 1.377(3) . ?
C5 C10 1.502(3) . ?
C6 C7 1.378(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.396(3) . ?
C7 C11 1.507(4) . ?
C8 C9 1.386(3) . ?
C8 H8 0.9500 . ?
C9 C12 1.500(3) . ?
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 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.515(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.526(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.543(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.519(3) . ?
C16 H16 1.0000 . ?
C17 C18 1.527(3) . ?
C17 H17 1.0000 . ?
C18 C19 1.517(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.523(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.494(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C27 1.388(3) . ?
C22 C23 1.395(3) . ?
C23 C24 1.401(3) . ?
C24 C25 1.393(3) . ?
C24 C29 1.505(3) . ?
C25 C26 1.390(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.389(3) . ?
C26 C28 1.508(3) . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 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
O1 Al1 O3 121.49(8) . . ?
O1 Al1 O2 103.15(9) . . ?
O3 Al1 O2 90.58(8) . . ?
O1 Al1 N1 109.84(7) . . ?
O3 Al1 N1 127.29(7) . . ?
O2 Al1 N1 88.88(7) . . ?
O1 Al1 N2 89.62(7) . . ?
O3 Al1 N2 88.04(6) . . ?
O2 Al1 N2 165.74(8) . . ?
N1 Al1 N2 80.73(6) . . ?
C1 O1 Al1 129.49(18) . . ?
C12 N1 C13 109.29(15) . . ?
C12 N1 C16 108.69(14) . . ?
C13 N1 C16 103.63(14) . . ?
C12 N1 Al1 107.43(11) . . ?
C13 N1 Al1 113.53(11) . . ?
C16 N1 Al1 114.13(11) . . ?
O1 C1 C3 111.5(2) . . ?
O1 C1 C2 107.8(3) . . ?
C3 C1 C2 112.7(3) . . ?
O1 C1 H1 108.2 . . ?
C3 C1 H1 108.2 . . ?
C2 C1 H1 108.2 . . ?
C4 O2 Al1 135.92(14) . . ?
C17 N2 C21 109.89(14) . . ?
C17 N2 C20 105.31(15) . . ?
C21 N2 C20 109.38(15) . . ?
C17 N2 Al1 108.02(11) . . ?
C21 N2 Al1 108.94(11) . . ?
C20 N2 Al1 115.19(12) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C23 O3 Al1 133.58(12) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O2 C4 C9 121.36(18) . . ?
O2 C4 C5 119.7(2) . . ?
C9 C4 C5 118.9(2) . . ?
C6 C5 C4 119.1(2) . . ?
C6 C5 C10 122.5(2) . . ?
C4 C5 C10 118.4(2) . . ?
C5 C6 C7 122.9(2) . . ?
C5 C6 H6 118.5 . . ?
C7 C6 H6 118.5 . . ?
C6 C7 C8 117.7(2) . . ?
C6 C7 C11 120.7(2) . . ?
C8 C7 C11 121.7(3) . . ?
C9 C8 C7 121.4(2) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C8 C9 C4 119.86(19) . . ?
C8 C9 C12 121.19(19) . . ?
C4 C9 C12 118.95(18) . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 N1 113.12(15) . . ?
C9 C12 H12A 109.0 . . ?
N1 C12 H12A 109.0 . . ?
C9 C12 H12B 109.0 . . ?
N1 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
N1 C13 C14 104.81(15) . . ?
N1 C13 H13A 110.8 . . ?
C14 C13 H13A 110.8 . . ?
N1 C13 H13B 110.8 . . ?
C14 C13 H13B 110.8 . . ?
H13A C13 H13B 108.9 . . ?
C13 C14 C15 104.88(16) . . ?
C13 C14 H14A 110.8 . . ?
C15 C14 H14A 110.8 . . ?
C13 C14 H14B 110.8 . . ?
C15 C14 H14B 110.8 . . ?
H14A C14 H14B 108.8 . . ?
C14 C15 C16 105.41(16) . . ?
C14 C15 H15A 110.7 . . ?
C16 C15 H15A 110.7 . . ?
C14 C15 H15B 110.7 . . ?
C16 C15 H15B 110.7 . . ?
H15A C15 H15B 108.8 . . ?
N1 C16 C17 110.00(15) . . ?
N1 C16 C15 106.99(15) . . ?
C17 C16 C15 114.42(17) . . ?
N1 C16 H16 108.4 . . ?
C17 C16 H16 108.4 . . ?
C15 C16 H16 108.4 . . ?
N2 C17 C16 109.13(15) . . ?
N2 C17 C18 103.57(16) . . ?
C16 C17 C18 120.43(17) . . ?
N2 C17 H17 107.7 . . ?
C16 C17 H17 107.7 . . ?
C18 C17 H17 107.7 . . ?
C19 C18 C17 103.77(18) . . ?
C19 C18 H18A 111.0 . . ?
C17 C18 H18A 111.0 . . ?
C19 C18 H18B 111.0 . . ?
C17 C18 H18B 111.0 . . ?
H18A C18 H18B 109.0 . . ?
C18 C19 C20 106.2(2) . . ?
C18 C19 H19A 110.5 . . ?
C20 C19 H19A 110.5 . . ?
C18 C19 H19B 110.5 . . ?
C20 C19 H19B 110.5 . . ?
H19A C19 H19B 108.7 . . ?
N2 C20 C19 106.43(18) . . ?
N2 C20 H20A 110.4 . . ?
C19 C20 H20A 110.4 . . ?
N2 C20 H20B 110.4 . . ?
C19 C20 H20B 110.4 . . ?
H20A C20 H20B 108.6 . . ?
C22 C21 N2 110.85(14) . . ?
C22 C21 H21A 109.5 . . ?
N2 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
N2 C21 H21B 109.5 . . ?
H21A C21 H21B 108.1 . . ?
C27 C22 C23 120.58(17) . . ?
C27 C22 C21 121.65(16) . . ?
C23 C22 C21 117.77(16) . . ?
O3 C23 C22 120.12(16) . . ?
O3 C23 C24 120.18(17) . . ?
C22 C23 C24 119.68(18) . . ?
C25 C24 C23 118.20(18) . . ?
C25 C24 C29 122.07(19) . . ?
C23 C24 C29 119.7(2) . . ?
C26 C25 C24 122.84(18) . . ?
C26 C25 H25 118.6 . . ?
C24 C25 H25 118.6 . . ?
C27 C26 C25 117.84(19) . . ?
C27 C26 C28 119.8(2) . . ?
C25 C26 C28 122.3(2) . . ?
C22 C27 C26 120.84(19) . . ?
C22 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C24 C29 H29A 109.5 . . ?
C24 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C24 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 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
O3 Al1 O1 C1 -100.0(2) . . . . ?
O2 Al1 O1 C1 -1.1(2) . . . . ?
N1 Al1 O1 C1 92.5(2) . . . . ?
N2 Al1 O1 C1 172.5(2) . . . . ?
Al1 O1 C1 C3 81.8(3) . . . . ?
Al1 O1 C1 C2 -153.9(2) . . . . ?
O1 Al1 O2 C4 127.9(2) . . . . ?
O3 Al1 O2 C4 -109.5(2) . . . . ?
N1 Al1 O2 C4 17.7(2) . . . . ?
N2 Al1 O2 C4 -25.2(5) . . . . ?
O1 Al1 O3 C23 -67.41(18) . . . . ?
O2 Al1 O3 C23 -173.25(17) . . . . ?
N1 Al1 O3 C23 97.73(17) . . . . ?
N2 Al1 O3 C23 20.95(16) . . . . ?
Al1 O2 C4 C9 2.9(4) . . . . ?
Al1 O2 C4 C5 -175.01(17) . . . . ?
O2 C4 C5 C6 175.15(19) . . . . ?
C9 C4 C5 C6 -2.8(3) . . . . ?
O2 C4 C5 C10 -1.6(3) . . . . ?
C9 C4 C5 C10 -179.58(19) . . . . ?
C4 C5 C6 C7 -0.6(3) . . . . ?
C10 C5 C6 C7 176.0(2) . . . . ?
C5 C6 C7 C8 2.4(3) . . . . ?
C5 C6 C7 C11 -176.2(2) . . . . ?
C6 C7 C8 C9 -0.8(3) . . . . ?
C11 C7 C8 C9 177.8(2) . . . . ?
C7 C8 C9 C4 -2.6(3) . . . . ?
C7 C8 C9 C12 177.91(19) . . . . ?
O2 C4 C9 C8 -173.6(2) . . . . ?
C5 C4 C9 C8 4.4(3) . . . . ?
O2 C4 C9 C12 6.0(3) . . . . ?
C5 C4 C9 C12 -176.10(17) . . . . ?
C8 C9 C12 N1 133.06(18) . . . . ?
C4 C9 C12 N1 -46.5(2) . . . . ?
C13 N1 C12 C9 -55.1(2) . . . . ?
C16 N1 C12 C9 -167.51(15) . . . . ?
Al1 N1 C12 C9 68.54(16) . . . . ?
C12 N1 C13 C14 -77.99(19) . . . . ?
C16 N1 C13 C14 37.7(2) . . . . ?
Al1 N1 C13 C14 162.10(14) . . . . ?
N1 C13 C14 C15 -35.1(2) . . . . ?
C13 C14 C15 C16 18.3(2) . . . . ?
C12 N1 C16 C17 -145.03(15) . . . . ?
C13 N1 C16 C17 98.81(17) . . . . ?
Al1 N1 C16 C17 -25.16(17) . . . . ?
C12 N1 C16 C15 90.13(18) . . . . ?
C13 N1 C16 C15 -26.0(2) . . . . ?
Al1 N1 C16 C15 -150.00(14) . . . . ?
C14 C15 C16 N1 4.7(2) . . . . ?
C14 C15 C16 C17 -117.37(19) . . . . ?
C21 N2 C17 C16 75.84(18) . . . . ?
C20 N2 C17 C16 -166.45(15) . . . . ?
Al1 N2 C17 C16 -42.88(16) . . . . ?
C21 N2 C17 C18 -154.72(16) . . . . ?
C20 N2 C17 C18 -37.01(19) . . . . ?
Al1 N2 C17 C18 86.56(15) . . . . ?
N1 C16 C17 N2 44.98(19) . . . . ?
C15 C16 C17 N2 165.42(15) . . . . ?
N1 C16 C17 C18 -74.5(2) . . . . ?
C15 C16 C17 C18 46.0(2) . . . . ?
N2 C17 C18 C19 37.1(2) . . . . ?
C16 C17 C18 C19 159.26(19) . . . . ?
C17 C18 C19 C20 -23.1(3) . . . . ?
C17 N2 C20 C19 22.6(2) . . . . ?
C21 N2 C20 C19 140.67(19) . . . . ?
Al1 N2 C20 C19 -96.27(19) . . . . ?
C18 C19 C20 N2 0.7(3) . . . . ?
C17 N2 C21 C22 174.44(15) . . . . ?
C20 N2 C21 C22 59.30(19) . . . . ?
Al1 N2 C21 C22 -67.40(16) . . . . ?
N2 C21 C22 C27 -126.04(17) . . . . ?
N2 C21 C22 C23 53.7(2) . . . . ?
Al1 O3 C23 C22 -42.8(2) . . . . ?
Al1 O3 C23 C24 138.83(16) . . . . ?
C27 C22 C23 O3 -177.92(16) . . . . ?
C21 C22 C23 O3 2.3(2) . . . . ?
C27 C22 C23 C24 0.5(3) . . . . ?
C21 C22 C23 C24 -179.27(16) . . . . ?
O3 C23 C24 C25 176.91(16) . . . . ?
C22 C23 C24 C25 -1.5(3) . . . . ?
O3 C23 C24 C29 -4.0(3) . . . . ?
C22 C23 C24 C29 177.57(17) . . . . ?
C23 C24 C25 C26 1.3(3) . . . . ?
C29 C24 C25 C26 -177.77(19) . . . . ?
C24 C25 C26 C27 0.0(3) . . . . ?
C24 C25 C26 C28 178.6(2) . . . . ?
C23 C22 C27 C26 0.8(3) . . . . ?
C21 C22 C27 C26 -179.42(17) . . . . ?
C25 C26 C27 C22 -1.1(3) . . . . ?
C28 C26 C27 C22 -179.67(19) . . . . ?
 
_refine_diff_density_max    0.354
_refine_diff_density_min   -0.223
_refine_diff_density_rms    0.041

#===END

data_Ti(3)(OiPr)2

_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C32 H48 N2 O4 Ti' 
_chemical_formula_weight          572.62

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'
 'O'  'O'   0.0492   0.0322
 '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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    13.7916(2)
_cell_length_b                    12.9946(2)
_cell_length_c                    17.5480(3)
_cell_angle_alpha                 90
_cell_angle_beta                  102.790(2)
_cell_angle_gamma                 90
_cell_volume                      3066.86(9)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used   11185
_cell_measurement_theta_min     4.2690
_cell_measurement_theta_max     71.8100
 
_exptl_crystal_description                'irregular'
_exptl_crystal_colour                     'clear light yellow'
_exptl_crystal_size_max                            0.3000
_exptl_crystal_size_mid                            0.1000
_exptl_crystal_size_min                            0.0500
_exptl_crystal_density_diffrn     1.240          
_exptl_crystal_F_000              1232
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_absorpt_coefficient_mu     2.657
_shelx_estimated_absorpt_T_min    0.619
_shelx_estimated_absorpt_T_max    0.879
_exptl_absorpt_correction_T_min                   0.71524
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_correction_type            'multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature       150(2)
_diffrn_ambient_environment 'N~2~'
_diffrn_source 'sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe 'x-ray'
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_radiation_monochromator 'mirror'
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector 'CCD plate'
_diffrn_detector_type 'EosS2'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number             20974
_diffrn_reflns_av_unetI/netI      0.0378
_diffrn_reflns_av_R_equivalents   0.0474
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          4.272
_diffrn_reflns_theta_max          66.573
_diffrn_reflns_theta_full         66.573
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              5415
_reflns_number_gt                 4952
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
_diffrn_measurement_method 'ω scans'
 
_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.
;
 
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution     SHELXS
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           
;
Two isopropyl groups show disorder.  The disorder was freely 
refined and then fixed for the final refinement cycle.  

Atoms C1 C2 C3 are 50:50 disordered with C1' C2' and C3', 
respectively. These two positions are well resolved enough to 
allow free refinement of the adps although C2' shows increased 
thermal motion in one direction resulting in a significantly 
elongated displacement parameter - it was not possible to model 
this further. 

Atoms C4 C5 and C6 are 80:20 disordered with C4' C5' and C6', 
respectively. The relatively close positioning of these two sites
and the low occupancy of the second position resulted in 
unreasonable adps.  EADP constraints were therefore applied to
the adps - the eadps of of C4 and C4'  were constrained to take
the same value, and C5, C6, C5' and C6' were constrained to take 
the same value.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1146P)²+1.2394P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      difmap
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          5415
_refine_ls_number_parameters      394
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0632
_refine_ls_R_factor_gt            0.0599
_refine_ls_wR_factor_ref          0.1698
_refine_ls_wR_factor_gt           0.1651
_refine_ls_goodness_of_fit_ref    1.037
_refine_ls_restrained_S_all       1.037
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.3382(5) 0.4567(5) 0.5582(4) 0.0381(13) Uani 0.5 1 d . . P A 1
H1 H 0.4049 0.4895 0.5628 0.046 Uiso 0.5 1 calc R U P A 1
C3 C 0.2866(7) 0.4562(6) 0.4720(5) 0.071(2) Uani 0.5 1 d . . P A 1
H3A H 0.2211 0.4238 0.4655 0.106 Uiso 0.5 1 calc R U P A 1
H3B H 0.3269 0.4173 0.4424 0.106 Uiso 0.5 1 calc R U P A 1
H3C H 0.2787 0.5271 0.4526 0.106 Uiso 0.5 1 calc R U P A 1
C2 C 0.3545(9) 0.3536(6) 0.5928(5) 0.081(3) Uani 0.5 1 d . . P A 1
H2A H 0.3901 0.3595 0.6476 0.122 Uiso 0.5 1 calc R U P A 1
H2B H 0.3941 0.3127 0.5640 0.122 Uiso 0.5 1 calc R U P A 1
H2C H 0.2902 0.3200 0.5901 0.122 Uiso 0.5 1 calc R U P A 1
C3' C 0.4102(6) 0.4725(5) 0.5197(5) 0.0649(19) Uani 0.5 1 d . . P A 2
H3'1 H 0.4486 0.4408 0.5676 0.097 Uiso 0.5 1 calc R U P A 2
H3'2 H 0.4309 0.5444 0.5170 0.097 Uiso 0.5 1 calc R U P A 2
H3'3 H 0.4220 0.4349 0.4742 0.097 Uiso 0.5 1 calc R U P A 2
C2' C 0.2694(9) 0.3596(7) 0.5329(8) 0.110(5) Uani 0.5 1 d . . P A 2
H2'1 H 0.2739 0.3165 0.4880 0.164 Uiso 0.5 1 calc R U P A 2
H2'2 H 0.2004 0.3615 0.5387 0.164 Uiso 0.5 1 calc R U P A 2
H2'3 H 0.3119 0.3307 0.5804 0.164 Uiso 0.5 1 calc R U P A 2
C1' C 0.3040(6) 0.4688(6) 0.5201(7) 0.0496(16) Uani 0.5 1 d . . P A 2
H1' H 0.2631 0.4988 0.4709 0.060 Uiso 0.5 1 calc R U P A 2
C4 C 0.0872(3) 0.5543(3) 0.6470(2) 0.0383(8) Uani 0.8 1 d . . P B 3
H4 H 0.1152 0.4898 0.6295 0.046 Uiso 0.8 1 calc R U P B 3
C5 C 0.0445(3) 0.5316(5) 0.7167(3) 0.0757(10) Uani 0.8 1 d . . P B 3
H5A H 0.0984 0.5147 0.7615 0.114 Uiso 0.8 1 calc R U P B 3
H5B H -0.0013 0.4731 0.7050 0.114 Uiso 0.8 1 calc R U P B 3
H5C H 0.0084 0.5921 0.7291 0.114 Uiso 0.8 1 calc R U P B 3
C6 C 0.0070(4) 0.5945(5) 0.5826(3) 0.0757(10) Uani 0.8 1 d . . P B 3
H6A H -0.0184 0.6594 0.5990 0.114 Uiso 0.8 1 calc R U P B 3
H6B H -0.0472 0.5442 0.5704 0.114 Uiso 0.8 1 calc R U P B 3
H6C H 0.0338 0.6065 0.5361 0.114 Uiso 0.8 1 calc R U P B 3
C5' C -0.0045(15) 0.6470(17) 0.6843(13) 0.0757(10) Uani 0.2 1 d . . P B 4
H5'1 H -0.0714 0.6192 0.6645 0.114 Uiso 0.2 1 calc R U P B 4
H5'2 H 0.0157 0.6348 0.7407 0.114 Uiso 0.2 1 calc R U P B 4
H5'3 H -0.0047 0.7211 0.6740 0.114 Uiso 0.2 1 calc R U P B 4
C6' C 0.0339(16) 0.572(2) 0.5535(14) 0.0757(10) Uani 0.2 1 d . . P B 4
H6'1 H -0.0342 0.5452 0.5436 0.114 Uiso 0.2 1 calc R U P B 4
H6'2 H 0.0348 0.6365 0.5248 0.114 Uiso 0.2 1 calc R U P B 4
H6'3 H 0.0772 0.5216 0.5361 0.114 Uiso 0.2 1 calc R U P B 4
C4' C 0.0714(14) 0.5918(13) 0.6417(12) 0.0383(8) Uani 0.2 1 d . . P B 4
H4' H 0.0761 0.5208 0.6642 0.046 Uiso 0.2 1 calc R U P B 4
Ti1 Ti 0.27517(3) 0.65298(3) 0.62636(3) 0.03333(18) Uani 1 1 d . . . . .
O1 O 0.28150(14) 0.52216(15) 0.59178(13) 0.0489(5) Uani 1 1 d . . . . .
N1 N 0.28083(14) 0.81183(15) 0.68754(11) 0.0284(4) Uani 1 1 d . . . . .
O2 O 0.16468(13) 0.62931(14) 0.66832(11) 0.0390(4) Uani 1 1 d . . . . .
N2 N 0.37054(15) 0.61760(15) 0.74812(13) 0.0342(4) Uani 1 1 d . . . . .
O3 O 0.20988(13) 0.72396(14) 0.53662(10) 0.0401(4) Uani 1 1 d . . . . .
O4 O 0.40432(12) 0.69401(15) 0.60605(10) 0.0380(4) Uani 1 1 d . . . . .
C7 C 0.18018(18) 0.8201(2) 0.51586(14) 0.0362(5) Uani 1 1 d . . . . .
C8 C 0.1051(2) 0.8356(2) 0.44809(15) 0.0423(6) Uani 1 1 d . . . . .
C9 C 0.0753(2) 0.9349(3) 0.42667(15) 0.0465(7) Uani 1 1 d . . . . .
H9 H 0.0238 0.9449 0.3814 0.056 Uiso 1 1 calc R U . . .
C10 C 0.1175(2) 1.0210(2) 0.46851(15) 0.0438(6) Uani 1 1 d . . . . .
C11 C 0.19083(19) 1.0039(2) 0.53590(14) 0.0377(5) Uani 1 1 d . . . . .
H11 H 0.2197 1.0612 0.5663 0.045 Uiso 1 1 calc R U . . .
C12 C 0.22312(18) 0.9050(2) 0.56003(14) 0.0339(5) Uani 1 1 d . . . . .
C13 C 0.0576(2) 0.7444(3) 0.40193(17) 0.0537(8) Uani 1 1 d . . . . .
H13A H -0.0002 0.7222 0.4216 0.081 Uiso 1 1 calc R U . . .
H13B H 0.1057 0.6879 0.4073 0.081 Uiso 1 1 calc R U . . .
H13C H 0.0363 0.7634 0.3467 0.081 Uiso 1 1 calc R U . . .
C14 C 0.0846(3) 1.1281(3) 0.44199(18) 0.0544(8) Uani 1 1 d . . . . .
H14A H 0.0958 1.1397 0.3894 0.082 Uiso 1 1 calc R U . . .
H14B H 0.1230 1.1784 0.4782 0.082 Uiso 1 1 calc R U . . .
H14C H 0.0137 1.1361 0.4411 0.082 Uiso 1 1 calc R U . . .
C15 C 0.30443(18) 0.89179(18) 0.63257(13) 0.0315(5) Uani 1 1 d . . . . .
H15A H 0.3667 0.8722 0.6170 0.038 Uiso 1 1 calc R U . . .
H15B H 0.3160 0.9585 0.6603 0.038 Uiso 1 1 calc R U . . .
C16 C 0.19158(18) 0.84688(18) 0.71629(14) 0.0318(5) Uani 1 1 d . . . . .
H16A H 0.1583 0.7875 0.7350 0.038 Uiso 1 1 calc R U . . .
H16B H 0.1433 0.8814 0.6738 0.038 Uiso 1 1 calc R U . . .
C17 C 0.22983(19) 0.9220(2) 0.78335(15) 0.0376(5) Uani 1 1 d . . . . .
H17A H 0.1957 0.9104 0.8266 0.045 Uiso 1 1 calc R U . . .
H17B H 0.2181 0.9940 0.7652 0.045 Uiso 1 1 calc R U . . .
C18 C 0.34191(19) 0.90067(18) 0.81050(14) 0.0338(5) Uani 1 1 d . . . . .
H18A H 0.3587 0.8810 0.8664 0.041 Uiso 1 1 calc R U . . .
H18B H 0.3810 0.9624 0.8033 0.041 Uiso 1 1 calc R U . . .
C19 C 0.36395(17) 0.81132(18) 0.75903(13) 0.0301(5) Uani 1 1 d . . . . .
H19 H 0.4276 0.8263 0.7429 0.036 Uiso 1 1 calc R U . . .
C20 C 0.37437(17) 0.70823(18) 0.80235(14) 0.0329(5) Uani 1 1 d . . . . .
H20 H 0.4421 0.7078 0.8376 0.040 Uiso 1 1 calc R U . . .
C21 C 0.3011(2) 0.6806(2) 0.85324(16) 0.0422(6) Uani 1 1 d . . . . .
H21A H 0.3159 0.7190 0.9032 0.051 Uiso 1 1 calc R U . . .
H21B H 0.2316 0.6942 0.8256 0.051 Uiso 1 1 calc R U . . .
C22 C 0.3204(2) 0.5656(2) 0.86626(18) 0.0480(7) Uani 1 1 d . . . . .
H22A H 0.3838 0.5528 0.9044 0.058 Uiso 1 1 calc R U . . .
H22B H 0.2655 0.5317 0.8847 0.058 Uiso 1 1 calc R U . . .
C23 C 0.3254(2) 0.5291(2) 0.78561(18) 0.0444(6) Uani 1 1 d . . . . .
H23A H 0.2581 0.5125 0.7547 0.053 Uiso 1 1 calc R U . . .
H23B H 0.3676 0.4669 0.7889 0.053 Uiso 1 1 calc R U . . .
C24 C 0.47272(19) 0.58264(19) 0.74396(17) 0.0383(5) Uani 1 1 d . . . . .
H24A H 0.4661 0.5207 0.7103 0.046 Uiso 1 1 calc R U . . .
H24B H 0.5082 0.5616 0.7971 0.046 Uiso 1 1 calc R U . . .
C25 C 0.53633(19) 0.65962(17) 0.71349(16) 0.0355(5) Uani 1 1 d . . . . .
C26 C 0.63494(19) 0.67575(19) 0.75208(17) 0.0401(6) Uani 1 1 d . . . . .
H26 H 0.6593 0.6449 0.8017 0.048 Uiso 1 1 calc R U . . .
C27 C 0.69841(19) 0.7361(2) 0.71939(18) 0.0436(6) Uani 1 1 d . . . . .
C28 C 0.6602(2) 0.78098(19) 0.64746(17) 0.0411(6) Uani 1 1 d . . . . .
H28 H 0.7031 0.8212 0.6239 0.049 Uiso 1 1 calc R U . . .
C29 C 0.56181(19) 0.76943(19) 0.60839(15) 0.0378(6) Uani 1 1 d . . . . .
C30 C 0.49888(18) 0.70723(18) 0.64186(15) 0.0342(5) Uani 1 1 d . . . . .
C31 C 0.5220(2) 0.8206(3) 0.53087(17) 0.0515(7) Uani 1 1 d . . . . .
H31A H 0.4791 0.8782 0.5379 0.077 Uiso 1 1 calc R U . . .
H31B H 0.4836 0.7706 0.4945 0.077 Uiso 1 1 calc R U . . .
H31C H 0.5776 0.8462 0.5097 0.077 Uiso 1 1 calc R U . . .
C32 C 0.8055(2) 0.7520(3) 0.7620(2) 0.0638(9) Uani 1 1 d . . . . .
H32A H 0.8395 0.7948 0.7301 0.096 Uiso 1 1 calc R U . . .
H32B H 0.8389 0.6851 0.7715 0.096 Uiso 1 1 calc R U . . .
H32C H 0.8073 0.7863 0.8120 0.096 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 O1 1.374(6) . ?
C1 C2 1.467(10) . ?
C1 C3 1.522(9) . ?
C3' C1' 1.467(10) . ?
C2' C1' 1.530(12) . ?
C1' O1 1.528(9) . ?
C4 O2 1.433(4) . ?
C4 C6 1.490(7) . ?
C4 C5 1.500(6) . ?
C5' C4' 1.59(3) . ?
C6' C4' 1.54(3) . ?
C4' O2 1.358(19) . ?
Ti1 O1 1.8136(18) . ?
Ti1 O2 1.8590(18) . ?
Ti1 O3 1.8745(19) . ?
Ti1 O4 1.9659(17) . ?
Ti1 N2 2.294(2) . ?
Ti1 N1 2.3200(19) . ?
N1 C19 1.500(3) . ?
N1 C16 1.501(3) . ?
N1 C15 1.502(3) . ?
N2 C24 1.498(3) . ?
N2 C20 1.508(3) . ?
N2 C23 1.524(3) . ?
O3 C7 1.340(3) . ?
O4 C30 1.328(3) . ?
C7 C12 1.403(4) . ?
C7 C8 1.408(4) . ?
C8 C9 1.381(4) . ?
C8 C13 1.502(4) . ?
C9 C10 1.393(5) . ?
C10 C11 1.394(4) . ?
C10 C14 1.505(4) . ?
C11 C12 1.394(4) . ?
C12 C15 1.508(3) . ?
C16 C17 1.530(3) . ?
C17 C18 1.539(4) . ?
C18 C19 1.542(3) . ?
C19 C20 1.531(3) . ?
C20 C21 1.531(3) . ?
C21 C22 1.527(4) . ?
C22 C23 1.508(4) . ?
C24 C25 1.505(4) . ?
C25 C30 1.394(4) . ?
C25 C26 1.394(4) . ?
C26 C27 1.390(4) . ?
C27 C28 1.384(4) . ?
C27 C32 1.514(4) . ?
C28 C29 1.387(4) . ?
C29 C30 1.406(4) . ?
C29 C31 1.504(4) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 C1 C2 115.9(6) . . ?
O1 C1 C3 104.1(5) . . ?
C2 C1 C3 113.8(6) . . ?
C3' C1' O1 111.9(7) . . ?
C3' C1' C2' 112.0(7) . . ?
O1 C1' C2' 100.0(6) . . ?
O2 C4 C6 110.2(3) . . ?
O2 C4 C5 109.0(3) . . ?
C6 C4 C5 109.1(4) . . ?
O2 C4' C6' 119.2(16) . . ?
O2 C4' C5' 110.4(14) . . ?
C6' C4' C5' 116.0(17) . . ?
O1 Ti1 O2 94.69(9) . . ?
O1 Ti1 O3 103.28(9) . . ?
O2 Ti1 O3 97.51(9) . . ?
O1 Ti1 O4 94.64(8) . . ?
O2 Ti1 O4 166.34(8) . . ?
O3 Ti1 O4 90.01(8) . . ?
O1 Ti1 N2 93.65(9) . . ?
O2 Ti1 N2 87.08(8) . . ?
O3 Ti1 N2 161.97(8) . . ?
O4 Ti1 N2 82.39(7) . . ?
O1 Ti1 N1 171.75(9) . . ?
O2 Ti1 N1 84.86(7) . . ?
O3 Ti1 N1 84.93(7) . . ?
O4 Ti1 N1 84.47(7) . . ?
N2 Ti1 N1 78.10(7) . . ?
C1 O1 Ti1 143.0(3) . . ?
C1' O1 Ti1 137.3(4) . . ?
C19 N1 C16 104.59(17) . . ?
C19 N1 C15 107.82(17) . . ?
C16 N1 C15 108.46(18) . . ?
C19 N1 Ti1 108.91(13) . . ?
C16 N1 Ti1 118.66(14) . . ?
C15 N1 Ti1 107.95(13) . . ?
C4' O2 Ti1 136.0(9) . . ?
C4 O2 Ti1 129.6(2) . . ?
C24 N2 C20 111.45(19) . . ?
C24 N2 C23 105.70(19) . . ?
C20 N2 C23 106.1(2) . . ?
C24 N2 Ti1 111.54(16) . . ?
C20 N2 Ti1 111.36(14) . . ?
C23 N2 Ti1 110.41(15) . . ?
C7 O3 Ti1 138.45(16) . . ?
C30 O4 Ti1 141.61(17) . . ?
O3 C7 C12 121.2(2) . . ?
O3 C7 C8 119.1(2) . . ?
C12 C7 C8 119.7(3) . . ?
C9 C8 C7 118.8(3) . . ?
C9 C8 C13 121.5(3) . . ?
C7 C8 C13 119.6(3) . . ?
C8 C9 C10 122.9(2) . . ?
C9 C10 C11 117.3(3) . . ?
C9 C10 C14 121.2(3) . . ?
C11 C10 C14 121.5(3) . . ?
C10 C11 C12 121.9(3) . . ?
C11 C12 C7 119.3(2) . . ?
C11 C12 C15 119.3(2) . . ?
C7 C12 C15 121.4(2) . . ?
N1 C15 C12 113.2(2) . . ?
N1 C16 C17 106.46(19) . . ?
C16 C17 C18 105.96(19) . . ?
C17 C18 C19 105.61(19) . . ?
N1 C19 C20 112.92(19) . . ?
N1 C19 C18 105.85(18) . . ?
C20 C19 C18 112.14(19) . . ?
N2 C20 C19 112.55(19) . . ?
N2 C20 C21 104.5(2) . . ?
C19 C20 C21 119.5(2) . . ?
C22 C21 C20 101.6(2) . . ?
C23 C22 C21 102.1(2) . . ?
C22 C23 N2 106.0(2) . . ?
N2 C24 C25 116.4(2) . . ?
C30 C25 C26 119.9(2) . . ?
C30 C25 C24 119.1(2) . . ?
C26 C25 C24 120.7(2) . . ?
C27 C26 C25 121.3(3) . . ?
C28 C27 C26 117.8(2) . . ?
C28 C27 C32 121.7(3) . . ?
C26 C27 C32 120.5(3) . . ?
C27 C28 C29 122.6(3) . . ?
C28 C29 C30 118.9(3) . . ?
C28 C29 C31 121.3(2) . . ?
C30 C29 C31 119.8(2) . . ?
O4 C30 C25 119.9(2) . . ?
O4 C30 C29 120.6(2) . . ?
C25 C30 C29 119.5(2) . . ?
 
_refine_diff_density_max    0.671
_refine_diff_density_min   -0.752
_refine_diff_density_rms    0.069