data_9406

# Crystallographer: Patrick J. Carroll

$ Compound 1

_audit_creation_date               2018-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_formula_moiety           'C34 H62 N P2 Sc Si2'
_chemical_formula_sum              'C34 H62 N P2 Sc Si2'
_chemical_formula_weight           647.92

loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Sc' 'Sc' 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'

loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     12.6597(15)
_cell_length_b                     14.6041(17)
_cell_length_c                     14.8346(18)
_cell_angle_alpha                  109.894(5)
_cell_angle_beta                   105.782(5)
_cell_angle_gamma                  108.149(5)
_cell_volume                       2220.6(5)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      9934
_cell_measurement_temperature      100
_cell_measurement_theta_max        27.48
_cell_measurement_theta_min        2.48
_shelx_estimated_absorpt_T_max     0.976
_shelx_estimated_absorpt_T_min     0.921
_exptl_absorpt_coefficient_mu      0.311
_exptl_absorpt_correction_T_max    0.7456
_exptl_absorpt_correction_T_min    0.6054
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     'TWINABS v2012/1'
_exptl_crystal_colour              'light yellow'
_exptl_crystal_density_diffrn      0.969
_exptl_crystal_description         plank
_exptl_crystal_F_000               704
_exptl_crystal_size_max            0.27
_exptl_crystal_size_mid            0.12
_exptl_crystal_size_min            0.08
_diffrn_reflns_av_R_equivalents    0.0776
_diffrn_reflns_av_unetI/netI       0.0574
_diffrn_reflns_Laue_measured_fraction_full  0.999
_diffrn_reflns_Laue_measured_fraction_max  0.993
_diffrn_reflns_limit_h_max         15
_diffrn_reflns_limit_h_min         -16
_diffrn_reflns_limit_k_max         17
_diffrn_reflns_limit_k_min         -18
_diffrn_reflns_limit_l_max         19
_diffrn_reflns_limit_l_min         0
_diffrn_reflns_number              77246
_diffrn_reflns_point_group_measured_fraction_full  0.999
_diffrn_reflns_point_group_measured_fraction_max  0.993
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.552
_diffrn_reflns_theta_min           1.611
_diffrn_ambient_temperature        100
_diffrn_measured_fraction_theta_full  0.999
_diffrn_measured_fraction_theta_max  0.993
_diffrn_measurement_device         'CCD area detector'
_diffrn_measurement_device_type    'Bruker APEXII'
_diffrn_measurement_method         'ω and φ scans'
_diffrn_radiation_monochromator    graphite
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed tube'
_reflns_number_gt                  8400
_reflns_number_total               10173
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'Bruker SAINT v8.34A'
_computing_data_collection         'Bruker APEX2 v2014.11-0'
_computing_data_reduction          'Bruker SAINT v8.34A'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max           0.572
_refine_diff_density_min           -0.446
_refine_diff_density_rms           0.057
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.058
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       377
_refine_ls_number_reflns           10173
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0572
_refine_ls_R_factor_gt             0.0433
_refine_ls_restrained_S_all        1.058
_refine_ls_shift/su_max            0.001
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0525P)²+0.8545P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1093
_refine_ls_wR_factor_ref           0.1155
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       direct
_refine_special_details
;
The data were corrected for the presence of disordered solvent using the
program SQUEEZE.
;

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
 Sc1 Sc 0.58108(3) 0.69197(3) 0.36179(3) 0.01822(9) Uani 1 1 d . . . . .
 P1 P 0.77212(5) 0.65250(4) 0.33060(4) 0.01879(11) Uani 1 1 d . . . . .
 P2 P 0.32942(5) 0.59895(4) 0.29171(4) 0.01970(11) Uani 1 1 d . . . . .
 Si1 Si 0.68488(6) 0.88497(5) 0.63169(5) 0.02411(13) Uani 1 1 d . . . . .
 Si2 Si 0.64003(6) 0.88451(5) 0.24065(5) 0.02491(13) Uani 1 1 d . . . . .
 N1 N 0.51071(15) 0.51745(13) 0.27083(13) 0.0195(3) Uani 1 1 d . . . . .
 C1 C 0.58575(18) 0.46956(15) 0.30089(15) 0.0188(4) Uani 1 1 d . . . . .
 C2 C 0.71398(18) 0.52306(15) 0.33264(15) 0.0192(4) Uani 1 1 d . . . . .
 C3 C 0.78917(19) 0.47703(16) 0.36593(16) 0.0216(4) Uani 1 1 d . . . . .
 H3 H 0.875037 0.514609 0.387987 0.026 Uiso 1 1 calc R . . . .
 C4 C 0.74257(19) 0.37896(16) 0.36772(17) 0.0227(4) Uani 1 1 d . . . . .
 C5 C 0.61618(19) 0.32709(16) 0.33743(17) 0.0234(4) Uani 1 1 d . . . . .
 H5 H 0.581881 0.260041 0.338890 0.028 Uiso 1 1 calc R . . . .
 C6 C 0.53996(19) 0.37111(16) 0.30541(16) 0.0218(4) Uani 1 1 d . . . . .
 H6 H 0.454691 0.333906 0.286022 0.026 Uiso 1 1 calc R . . . .
 C7 C 0.8248(2) 0.32972(18) 0.40115(19) 0.0294(5) Uani 1 1 d . . . . .
 H7a H 0.808386 0.264934 0.339457 0.044 Uiso 1 1 calc GR . . . .
 H7b H 0.808748 0.309209 0.454216 0.044 Uiso 1 1 calc GR . . . .
 H7c H 0.910813 0.383015 0.431508 0.044 Uiso 1 1 calc GR . . . .
 C8 C 0.39343(18) 0.44643(15) 0.18648(16) 0.0197(4) Uani 1 1 d . . . . .
 C9 C 0.29546(18) 0.47480(16) 0.18040(16) 0.0202(4) Uani 1 1 d . . . . .
 C10 C 0.17998(19) 0.40626(17) 0.09491(17) 0.0249(4) Uani 1 1 d . . . . .
 H10 H 0.115662 0.427117 0.092176 0.030 Uiso 1 1 calc R . . . .
 C11 C 0.1563(2) 0.30912(18) 0.01423(17) 0.0274(5) Uani 1 1 d . . . . .
 C12 C 0.2532(2) 0.28187(17) 0.02078(17) 0.0266(4) Uani 1 1 d . . . . .
 H12 H 0.239738 0.215719 -0.033348 0.032 Uiso 1 1 calc R . . . .
 C13 C 0.36872(19) 0.34841(16) 0.10398(16) 0.0233(4) Uani 1 1 d . . . . .
 H13 H 0.432521 0.327088 0.105083 0.028 Uiso 1 1 calc R . . . .
 C14 C 0.0309(2) 0.2353(2) -0.0772(2) 0.0375(6) Uani 1 1 d . . . . .
 H14a H 0.032818 0.171093 -0.125629 0.056 Uiso 1 1 calc R . . . .
 H14b H -0.029654 0.212360 -0.050172 0.056 Uiso 1 1 calc R . . . .
 H14c H 0.008466 0.274626 -0.115053 0.056 Uiso 1 1 calc R . . . .
 C15 C 0.77920(19) 0.61800(17) 0.20030(17) 0.0231(4) Uani 1 1 d . . . . .
 H15 H 0.809534 0.687325 0.195457 0.028 Uiso 1 1 calc R . . . .
 C16 C 0.6509(2) 0.54271(19) 0.11005(17) 0.0302(5) Uani 1 1 d . . . . .
 H16a H 0.620085 0.472245 0.110007 0.045 Uiso 1 1 calc GR . . . .
 H16b H 0.654829 0.532106 0.042391 0.045 Uiso 1 1 calc GR . . . .
 H16c H 0.595524 0.575572 0.119978 0.045 Uiso 1 1 calc GR . . . .
 C17 C 0.8677(2) 0.5686(2) 0.18629(19) 0.0336(5) Uani 1 1 d . . . . .
 H17a H 0.951068 0.620970 0.240185 0.050 Uiso 1 1 calc GR . . . .
 H17b H 0.865779 0.551074 0.115780 0.050 Uiso 1 1 calc GR . . . .
 H17c H 0.842825 0.502009 0.193936 0.050 Uiso 1 1 calc GR . . . .
 C18 C 0.93351(18) 0.72767(16) 0.43016(16) 0.0217(4) Uani 1 1 d . . . . .
 H18 H 0.975366 0.680433 0.413668 0.026 Uiso 1 1 calc R . . . .
 C19 C 0.9996(2) 0.83183(17) 0.42492(19) 0.0295(5) Uani 1 1 d . . . . .
 H19a H 0.994271 0.813290 0.353293 0.044 Uiso 1 1 calc GR . . . .
 H19b H 1.086009 0.868946 0.475534 0.044 Uiso 1 1 calc GR . . . .
 H19c H 0.960966 0.879922 0.442574 0.044 Uiso 1 1 calc GR . . . .
 C20 C 0.9402(2) 0.75399(18) 0.54095(17) 0.0263(4) Uani 1 1 d . . . . .
 H20a H 0.899186 0.800074 0.558312 0.039 Uiso 1 1 calc GR . . . .
 H20b H 1.026244 0.792533 0.592432 0.039 Uiso 1 1 calc GR . . . .
 H20c H 0.899303 0.686266 0.543220 0.039 Uiso 1 1 calc GR . . . .
 C21 C 0.2273(2) 0.65306(17) 0.23883(18) 0.0250(4) Uani 1 1 d . . . . .
 H21 H 0.140601 0.595383 0.203875 0.030 Uiso 1 1 calc R . . . .
 C22 C 0.2576(2) 0.6825(2) 0.1565(2) 0.0350(5) Uani 1 1 d . . . . .
 H22a H 0.342611 0.738668 0.189559 0.052 Uiso 1 1 calc GR . . . .
 H22b H 0.202202 0.710148 0.128346 0.052 Uiso 1 1 calc GR . . . .
 H22c H 0.247443 0.617649 0.098680 0.052 Uiso 1 1 calc GR . . . .
 C23 C 0.2399(2) 0.75156(19) 0.3300(2) 0.0332(5) Uani 1 1 d . . . . .
 H23a H 0.213698 0.728906 0.378449 0.050 Uiso 1 1 calc GR . . . .
 H23b H 0.188444 0.782160 0.301747 0.050 Uiso 1 1 calc GR . . . .
 H23c H 0.325792 0.806750 0.368135 0.050 Uiso 1 1 calc GR . . . .
 C24 C 0.2702(2) 0.55142(17) 0.37706(17) 0.0236(4) Uani 1 1 d . . . . .
 H24 H 0.299205 0.617222 0.445359 0.028 Uiso 1 1 calc R . . . .
 C25 C 0.1303(2) 0.49267(19) 0.3321(2) 0.0321(5) Uani 1 1 d . . . . .
 H25a H 0.096171 0.542489 0.323480 0.048 Uiso 1 1 calc GR . . . .
 H25b H 0.106667 0.468449 0.380725 0.048 Uiso 1 1 calc GR . . . .
 H25c H 0.098272 0.429455 0.263198 0.048 Uiso 1 1 calc GR . . . .
 C26 C 0.3250(2) 0.47849(17) 0.40277(18) 0.0259(4) Uani 1 1 d . . . . .
 H26a H 0.292624 0.410097 0.338394 0.039 Uiso 1 1 calc GR . . . .
 H26b H 0.302878 0.462964 0.456156 0.039 Uiso 1 1 calc GR . . . .
 H26c H 0.414525 0.515811 0.430176 0.039 Uiso 1 1 calc GR . . . .
 C27 C 0.63427(19) 0.74417(16) 0.53288(16) 0.0235(4) Uani 1 1 d . . . . .
 H27a H 0.563209 0.697536 0.538630 0.028 Uiso 1 1 calc R . . . .
 H27b H 0.701046 0.724535 0.556849 0.028 Uiso 1 1 calc R . . . .
 C28 C 0.8365(2) 0.97963(18) 0.64748(19) 0.0333(5) Uani 1 1 d . . . . .
 H28a H 0.901245 0.963795 0.682258 0.050 Uiso 1 1 calc GR . . . .
 H28b H 0.854469 1.055059 0.690724 0.050 Uiso 1 1 calc GR . . . .
 H28c H 0.832891 0.969390 0.577711 0.050 Uiso 1 1 calc GR . . . .
 C29 C 0.7074(2) 0.9039(2) 0.76844(19) 0.0376(6) Uani 1 1 d . . . . .
 H29a H 0.627376 0.870921 0.768951 0.056 Uiso 1 1 calc GR . . . .
 H29b H 0.749300 0.981759 0.818279 0.056 Uiso 1 1 calc GR . . . .
 H29c H 0.757190 0.868775 0.789429 0.056 Uiso 1 1 calc GR . . . .
 C30 C 0.5688(2) 0.93410(19) 0.5896(2) 0.0345(5) Uani 1 1 d . . . . .
 H30a H 0.566952 0.940651 0.525683 0.052 Uiso 1 1 calc GR . . . .
 H30b H 0.591359 1.005288 0.646418 0.052 Uiso 1 1 calc GR . . . .
 H30c H 0.487610 0.882013 0.574826 0.052 Uiso 1 1 calc GR . . . .
 C31 C 0.6053(2) 0.83514(17) 0.33263(18) 0.0260(4) Uani 1 1 d . . . . .
 H31a H 0.528003 0.840155 0.328113 0.031 Uiso 1 1 calc R . . . .
 H31b H 0.668554 0.896158 0.402180 0.031 Uiso 1 1 calc R . . . .
 C32 C 0.8040(2) 0.92220(19) 0.26294(19) 0.0336(5) Uani 1 1 d . . . . .
 H32a H 0.857910 0.974890 0.337313 0.050 Uiso 1 1 calc GR . . . .
 H32b H 0.822696 0.954554 0.217765 0.050 Uiso 1 1 calc GR . . . .
 H32c H 0.817245 0.856856 0.245414 0.050 Uiso 1 1 calc GR . . . .
 C33 C 0.6208(3) 1.0112(2) 0.2591(3) 0.0512(8) Uani 1 1 d . . . . .
 H33a H 0.534194 0.994478 0.240349 0.077 Uiso 1 1 calc GR . . . .
 H33b H 0.648111 1.038337 0.213443 0.077 Uiso 1 1 calc GR . . . .
 H33c H 0.670091 1.066842 0.333170 0.077 Uiso 1 1 calc GR . . . .
 C34 C 0.5405(2) 0.7812(2) 0.0987(2) 0.0395(6) Uani 1 1 d . . . . .
 H34a H 0.554397 0.716269 0.084084 0.059 Uiso 1 1 calc GR . . . .
 H34b H 0.561005 0.811962 0.052940 0.059 Uiso 1 1 calc GR . . . .
 H34c H 0.454185 0.761199 0.084731 0.059 Uiso 1 1 calc GR . . . .


loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Sc1 P1 2.7733(7) . ?
 Sc1 P2 2.7599(7) . ?
 Sc1 N1 2.1683(16) . ?
 Sc1 C27 2.216(2) . ?
 Sc1 C31 2.223(2) . ?
 P1 C2 1.817(2) . ?
 P1 C15 1.860(2) . ?
 P1 C18 1.849(2) . ?
 P2 C9 1.814(2) . ?
 P2 C21 1.849(2) . ?
 P2 C24 1.854(2) . ?
 Si1 C27 1.845(2) . ?
 Si1 C28 1.879(2) . ?
 Si1 C29 1.878(2) . ?
 Si1 C30 1.878(2) . ?
 Si2 C31 1.837(2) . ?
 Si2 C32 1.875(3) . ?
 Si2 C33 1.879(2) . ?
 Si2 C34 1.873(3) . ?
 N1 C1 1.409(2) . ?
 N1 C8 1.412(3) . ?
 C1 C2 1.418(3) . ?
 C1 C6 1.405(3) . ?
 C2 C3 1.404(3) . ?
 C3 C4 1.381(3) . ?
 C4 C5 1.399(3) . ?
 C4 C7 1.509(3) . ?
 C5 C6 1.384(3) . ?
 C8 C9 1.415(3) . ?
 C8 C13 1.402(3) . ?
 C9 C10 1.401(3) . ?
 C10 C11 1.385(3) . ?
 C11 C12 1.391(3) . ?
 C11 C14 1.513(3) . ?
 C12 C13 1.387(3) . ?
 C15 C16 1.531(3) . ?
 C15 C17 1.532(3) . ?
 C18 C19 1.531(3) . ?
 C18 C20 1.527(3) . ?
 C21 C22 1.528(3) . ?
 C21 C23 1.529(3) . ?
 C24 C25 1.530(3) . ?
 C24 C26 1.534(3) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 P2 Sc1 P1 143.14(2) . . ?
 N1 Sc1 P1 72.50(5) . . ?
 N1 Sc1 P2 71.99(5) . . ?
 N1 Sc1 C27 112.11(7) . . ?
 N1 Sc1 C31 138.36(8) . . ?
 C27 Sc1 P1 103.22(6) . . ?
 C27 Sc1 P2 98.90(6) . . ?
 C27 Sc1 C31 109.39(8) . . ?
 C31 Sc1 P1 101.37(6) . . ?
 C31 Sc1 P2 98.55(6) . . ?
 C2 P1 Sc1 92.09(6) . . ?
 C2 P1 C15 104.76(9) . . ?
 C2 P1 C18 104.87(9) . . ?
 C15 P1 Sc1 120.55(7) . . ?
 C18 P1 Sc1 124.62(7) . . ?
 C18 P1 C15 105.54(9) . . ?
 C9 P2 Sc1 97.01(7) . . ?
 C9 P2 C21 105.89(10) . . ?
 C9 P2 C24 104.18(9) . . ?
 C21 P2 Sc1 125.59(7) . . ?
 C21 P2 C24 105.36(10) . . ?
 C24 P2 Sc1 115.89(7) . . ?
 C27 Si1 C28 111.14(10) . . ?
 C27 Si1 C29 114.95(10) . . ?
 C27 Si1 C30 110.10(11) . . ?
 C29 Si1 C28 105.40(11) . . ?
 C30 Si1 C28 108.42(12) . . ?
 C30 Si1 C29 106.49(12) . . ?
 C31 Si2 C32 110.79(11) . . ?
 C31 Si2 C33 112.56(11) . . ?
 C31 Si2 C34 112.59(11) . . ?
 C32 Si2 C33 105.54(13) . . ?
 C34 Si2 C32 107.97(11) . . ?
 C34 Si2 C33 107.02(14) . . ?
 C1 N1 Sc1 117.62(12) . . ?
 C1 N1 C8 116.79(15) . . ?
 C8 N1 Sc1 125.52(12) . . ?
 N1 C1 C2 120.13(17) . . ?
 C6 C1 N1 122.73(18) . . ?
 C6 C1 C2 117.08(17) . . ?
 C1 C2 P1 116.43(14) . . ?
 C3 C2 P1 123.49(15) . . ?
 C3 C2 C1 120.06(18) . . ?
 C4 C3 C2 122.24(19) . . ?
 C3 C4 C5 117.47(18) . . ?
 C3 C4 C7 121.26(19) . . ?
 C5 C4 C7 121.28(18) . . ?
 C6 C5 C4 121.59(19) . . ?
 C5 C6 C1 121.53(19) . . ?
 N1 C8 C9 120.09(17) . . ?
 C13 C8 N1 122.91(17) . . ?
 C13 C8 C9 116.95(18) . . ?
 C8 C9 P2 115.48(15) . . ?
 C10 C9 P2 124.19(15) . . ?
 C10 C9 C8 120.26(18) . . ?
 C11 C10 C9 122.29(19) . . ?
 C10 C11 C12 117.08(19) . . ?
 C10 C11 C14 121.8(2) . . ?
 C12 C11 C14 121.1(2) . . ?
 C13 C12 C11 122.0(2) . . ?
 C12 C13 C8 121.44(19) . . ?
 C16 C15 P1 110.52(14) . . ?
 C16 C15 C17 110.47(18) . . ?
 C17 C15 P1 113.70(15) . . ?
 C19 C18 P1 110.32(14) . . ?
 C20 C18 P1 110.61(14) . . ?
 C20 C18 C19 110.69(17) . . ?
 C22 C21 P2 110.22(14) . . ?
 C22 C21 C23 111.40(19) . . ?
 C23 C21 P2 109.40(15) . . ?
 C25 C24 P2 114.61(15) . . ?
 C25 C24 C26 109.75(18) . . ?
 C26 C24 P2 110.39(14) . . ?
 Si1 C27 Sc1 123.71(10) . . ?
 Si2 C31 Sc1 139.84(11) . . ?

