#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/20/4102092.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4102092
loop_
_publ_author_name
'Benjamin F. Wicker'
'Jennifer Scott'
'José G. Andino'
'Xinfeng Gao'
'Hyunsoo Park'
'Maren Pink'
'Daniel J. Mindiola'
_publ_section_title
;
 Phosphinidene Complexes of Scandium: Powerful PAr Group-Transfer Vehicles
 to Organic and Inorganic Substrates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3691
_journal_page_last               3693
_journal_paper_doi               10.1021/ja100214e
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
'(C26 H40 N P2) (C24 H25 P) (C4 H10 O2) Br Li Sc, 0.5(C4 H10 O) '
_chemical_formula_sum            'C56 H80 Br Li N O2.5 P3 Sc'
_chemical_formula_weight         1031.93
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8898(12)
_cell_length_b                   21.318(3)
_cell_length_c                   22.944(3)
_cell_measurement_reflns_used    2433
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      1.30
_cell_volume                     5815.5(13)
_computing_cell_refinement       'APEX 2'
_computing_data_collection       'APEX 2 (Bruker-AXS, 2009)'
_computing_data_reduction        'APEX 2'
_computing_molecular_graphics    'APEX 2'
_computing_publication_material  'APEX 2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 53.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  kappa
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35804
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.30
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker APEX II'
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  0.9548
_exptl_absorpt_correction_T_min  0.8961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         8362
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0830P)²+4.9419P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1510
_reflns_number_gt                6709
_reflns_number_total             8362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja100214e_si_003.cif
_cod_data_source_block           new
_cod_original_cell_volume        5815.7(11)
_cod_original_formula_sum        'C56 H80 Br Li N O2.50 P3 Sc'
_cod_database_code               4102092
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.98200(7) 0.37907(3) 0.23957(3) 0.0476(2) Uani 1 1 d . . .
Sc1 Sc 0.79448(9) 0.34729(5) 0.18900(5) 0.0189(3) Uani 1 1 d . . .
N1 N 0.7205(4) 0.2565(2) 0.17366(19) 0.0204(11) Uani 1 1 d . . .
P1 P 0.71637(15) 0.30331(7) 0.29268(6) 0.0255(4) Uani 1 1 d . . .
P2 P 0.89812(13) 0.29731(7) 0.09552(7) 0.0207(4) Uani 1 1 d . . .
C1 C 0.7968(7) 0.2390(3) 0.3286(3) 0.047(2) Uani 1 1 d . . .
H1 H 0.8517 0.2595 0.3556 0.056 Uiso 1 1 calc R . .
C2 C 0.7260(8) 0.1951(4) 0.3653(4) 0.065(3) Uani 1 1 d . . .
H2A H 0.7740 0.1622 0.3817 0.098 Uiso 1 1 calc R . .
H2B H 0.6677 0.1759 0.3409 0.098 Uiso 1 1 calc R . .
H2C H 0.6905 0.2188 0.3969 0.098 Uiso 1 1 calc R . .
C3 C 0.8619(9) 0.2029(5) 0.2873(4) 0.082(3) Uani 1 1 d . . .
H3A H 0.9082 0.1723 0.3083 0.123 Uiso 1 1 calc R . .
H3B H 0.9108 0.2311 0.2650 0.123 Uiso 1 1 calc R . .
H3C H 0.8111 0.1809 0.2607 0.123 Uiso 1 1 calc R . .
C4 C 0.6615(6) 0.3482(3) 0.3545(3) 0.0420(18) Uani 1 1 d . . .
H4 H 0.6121 0.3199 0.3781 0.050 Uiso 1 1 calc R . .
C5 C 0.5943(7) 0.3993(4) 0.3338(3) 0.053(2) Uani 1 1 d . . .
H5A H 0.5568 0.4197 0.3668 0.080 Uiso 1 1 calc R . .
H5B H 0.5375 0.3835 0.3065 0.080 Uiso 1 1 calc R . .
H5C H 0.6425 0.4298 0.3138 0.080 Uiso 1 1 calc R . .
C6 C 0.7579(9) 0.3696(5) 0.3929(4) 0.086(3) Uani 1 1 d . . .
H6A H 0.7288 0.3964 0.4241 0.129 Uiso 1 1 calc R . .
H6B H 0.8120 0.3933 0.3694 0.129 Uiso 1 1 calc R . .
H6C H 0.7953 0.3329 0.4099 0.129 Uiso 1 1 calc R . .
C7 C 0.5974(5) 0.2654(2) 0.2585(3) 0.0211(13) Uani 1 1 d . . .
C8 C 0.4913(6) 0.2585(3) 0.2829(3) 0.0264(15) Uani 1 1 d . . .
H8 H 0.4806 0.2720 0.3219 0.032 Uiso 1 1 calc R . .
C9 C 0.3991(5) 0.2329(3) 0.2535(3) 0.0257(15) Uani 1 1 d . . .
C10 C 0.2867(6) 0.2261(3) 0.2814(3) 0.0391(17) Uani 1 1 d . . .
H10A H 0.2283 0.2407 0.2545 0.059 Uiso 1 1 calc R . .
H10B H 0.2843 0.2512 0.3172 0.059 Uiso 1 1 calc R . .
H10C H 0.2736 0.1819 0.2910 0.059 Uiso 1 1 calc R . .
C11 C 0.4184(6) 0.2173(3) 0.1956(3) 0.0268(15) Uani 1 1 d . . .
H11 H 0.3576 0.2016 0.1730 0.032 Uiso 1 1 calc R . .
C12 C 0.5220(5) 0.2236(2) 0.1695(2) 0.0207(14) Uani 1 1 d . . .
H12 H 0.5313 0.2112 0.1300 0.025 Uiso 1 1 calc R . .
C13 C 0.6128(5) 0.2477(2) 0.1998(2) 0.0179(13) Uani 1 1 d . . .
C14 C 0.7648(5) 0.2054(3) 0.1422(2) 0.0200(13) Uani 1 1 d . . .
C15 C 0.7274(6) 0.1434(3) 0.1479(3) 0.0258(14) Uani 1 1 d . . .
H15 H 0.6666 0.1343 0.1734 0.031 Uiso 1 1 calc R . .
C16 C 0.7778(6) 0.0952(3) 0.1170(3) 0.0279(15) Uani 1 1 d . . .
H16 H 0.7509 0.0536 0.1221 0.033 Uiso 1 1 calc R . .
C17 C 0.8666(5) 0.1057(3) 0.0786(3) 0.0281(15) Uani 1 1 d . . .
C18 C 0.9222(6) 0.0510(3) 0.0469(3) 0.0402(18) Uani 1 1 d . . .
H18A H 0.8640 0.0230 0.0315 0.060 Uiso 1 1 calc R . .
H18B H 0.9702 0.0279 0.0741 0.060 Uiso 1 1 calc R . .
H18C H 0.9680 0.0671 0.0147 0.060 Uiso 1 1 calc R . .
C19 C 0.9028(5) 0.1669(3) 0.0727(3) 0.0260(15) Uani 1 1 d . . .
H19 H 0.9627 0.1759 0.0466 0.031 Uiso 1 1 calc R . .
C20 C 0.8546(5) 0.2159(3) 0.1038(3) 0.0234(14) Uani 1 1 d . . .
C21 C 1.0511(5) 0.2953(3) 0.0810(3) 0.0324(16) Uani 1 1 d . . .
H21 H 1.0636 0.2688 0.0457 0.039 Uiso 1 1 calc R . .
C22 C 1.0926(6) 0.3615(3) 0.0671(4) 0.053(2) Uani 1 1 d . . .
H22A H 1.1741 0.3606 0.0608 0.079 Uiso 1 1 calc R . .
H22B H 1.0751 0.3895 0.0997 0.079 Uiso 1 1 calc R . .
H22C H 1.0553 0.3767 0.0317 0.079 Uiso 1 1 calc R . .
C23 C 1.1153(6) 0.2657(4) 0.1312(3) 0.047(2) Uani 1 1 d . . .
H23A H 1.1961 0.2671 0.1229 0.070 Uiso 1 1 calc R . .
H23B H 1.0914 0.2220 0.1359 0.070 Uiso 1 1 calc R . .
H23C H 1.0997 0.2889 0.1672 0.070 Uiso 1 1 calc R . .
C24 C 0.8329(6) 0.3216(3) 0.0258(3) 0.0298(16) Uani 1 1 d . . .
H24 H 0.8457 0.3677 0.0215 0.036 Uiso 1 1 calc R . .
C25 C 0.7054(6) 0.3115(3) 0.0300(3) 0.0324(16) Uani 1 1 d . . .
H25A H 0.6693 0.3270 -0.0056 0.049 Uiso 1 1 calc R . .
H25B H 0.6760 0.3344 0.0637 0.049 Uiso 1 1 calc R . .
H25C H 0.6896 0.2666 0.0345 0.049 Uiso 1 1 calc R . .
C26 C 0.8817(8) 0.2905(4) -0.0277(3) 0.054(2) Uani 1 1 d . . .
H26A H 0.8411 0.3048 -0.0624 0.081 Uiso 1 1 calc R . .
H26B H 0.8743 0.2448 -0.0241 0.081 Uiso 1 1 calc R . .
H26C H 0.9614 0.3015 -0.0312 0.081 Uiso 1 1 calc R . .
P3 P 0.72741(14) 0.44604(7) 0.15626(7) 0.0216(4) Uani 1 1 d . . .
C27 C 0.6370(5) 0.4983(3) 0.1144(3) 0.0199(14) Uani 1 1 d . . .
C28 C 0.6787(5) 0.5342(3) 0.0665(3) 0.0257(15) Uani 1 1 d . . .
C29 C 0.6074(6) 0.5732(3) 0.0351(3) 0.0331(17) Uani 1 1 d . . .
H29 H 0.6369 0.5965 0.0033 0.040 Uiso 1 1 calc R . .
C30 C 0.4949(6) 0.5792(3) 0.0488(3) 0.0406(18) Uani 1 1 d . . .
H30 H 0.4469 0.6059 0.0268 0.049 Uiso 1 1 calc R . .
C31 C 0.4545(6) 0.5453(3) 0.0955(3) 0.0367(17) Uani 1 1 d . . .
H31 H 0.3772 0.5490 0.1054 0.044 Uiso 1 1 calc R . .
C32 C 0.5220(6) 0.5061(3) 0.1287(3) 0.0235(14) Uani 1 1 d . . .
C33 C 0.7990(6) 0.5330(3) 0.0487(3) 0.0272(15) Uani 1 1 d . . .
C34 C 0.8323(6) 0.4976(3) 0.0006(3) 0.0278(16) Uani 1 1 d . . .
C35 C 0.9453(6) 0.4987(3) -0.0171(3) 0.0364(18) Uani 1 1 d . . .
H35 H 0.9681 0.4736 -0.0492 0.044 Uiso 1 1 calc R . .
C36 C 1.0235(6) 0.5351(4) 0.0108(3) 0.0427(19) Uani 1 1 d . . .
C37 C 0.9887(6) 0.5720(3) 0.0578(3) 0.0382(18) Uani 1 1 d . . .
H37 H 1.0421 0.5979 0.0770 0.046 Uiso 1 1 calc R . .
C38 C 0.8789(6) 0.5718(3) 0.0770(3) 0.0282(15) Uani 1 1 d . . .
C39 C 0.7474(6) 0.4609(3) -0.0332(3) 0.0400(19) Uani 1 1 d . . .
H39A H 0.6976 0.4387 -0.0062 0.060 Uiso 1 1 calc R . .
H39B H 0.7860 0.4305 -0.0582 0.060 Uiso 1 1 calc R . .
H39C H 0.7028 0.4895 -0.0574 0.060 Uiso 1 1 calc R . .
C40 C 1.1445(7) 0.5354(5) -0.0088(4) 0.072(3) Uani 1 1 d . . .
H40A H 1.1857 0.5682 0.0122 0.108 Uiso 1 1 calc R . .
H40B H 1.1480 0.5436 -0.0507 0.108 Uiso 1 1 calc R . .
H40C H 1.1787 0.4945 -0.0004 0.108 Uiso 1 1 calc R . .
C41 C 0.8410(6) 0.6136(3) 0.1263(3) 0.0407(18) Uani 1 1 d . . .
H41A H 0.9066 0.6338 0.1440 0.061 Uiso 1 1 calc R . .
H41B H 0.8018 0.5884 0.1556 0.061 Uiso 1 1 calc R . .
H41C H 0.7899 0.6458 0.1111 0.061 Uiso 1 1 calc R . .
C42 C 0.4667(5) 0.4758(3) 0.1792(3) 0.0256(15) Uani 1 1 d . . .
C43 C 0.4133(5) 0.4170(3) 0.1743(3) 0.0239(15) Uani 1 1 d . . .
C44 C 0.3492(5) 0.3950(3) 0.2201(3) 0.0295(16) Uani 1 1 d . . .
H44 H 0.3103 0.3563 0.2158 0.035 Uiso 1 1 calc R . .
C45 C 0.3395(6) 0.4274(3) 0.2721(3) 0.0315(16) Uani 1 1 d . . .
C46 C 0.3914(6) 0.4849(3) 0.2759(3) 0.0366(17) Uani 1 1 d . . .
H46 H 0.3830 0.5084 0.3108 0.044 Uiso 1 1 calc R . .
C47 C 0.4551(6) 0.5100(3) 0.2314(3) 0.0315(16) Uani 1 1 d . . .
C48 C 0.4238(6) 0.3808(3) 0.1189(3) 0.0343(16) Uani 1 1 d . . .
H48A H 0.3827 0.3411 0.1225 0.052 Uiso 1 1 calc R . .
H48B H 0.5033 0.3721 0.1111 0.052 Uiso 1 1 calc R . .
H48C H 0.3922 0.4053 0.0867 0.052 Uiso 1 1 calc R . .
C49 C 0.2707(6) 0.4010(3) 0.3221(3) 0.0402(18) Uani 1 1 d . . .
H49A H 0.2459 0.4353 0.3474 0.060 Uiso 1 1 calc R . .
H49B H 0.3169 0.3716 0.3446 0.060 Uiso 1 1 calc R . .
H49C H 0.2048 0.3790 0.3065 0.060 Uiso 1 1 calc R . .
C50 C 0.5111(7) 0.5716(3) 0.2384(3) 0.051(2) Uani 1 1 d . . .
H50A H 0.5848 0.5706 0.2193 0.076 Uiso 1 1 calc R . .
H50B H 0.5209 0.5806 0.2800 0.076 Uiso 1 1 calc R . .
H50C H 0.4646 0.6044 0.2206 0.076 Uiso 1 1 calc R . .
Li1 Li 0.9054(10) 0.4840(5) 0.2022(6) 0.042(3) Uani 1 1 d . . .
O1 O 0.8860(7) 0.5377(3) 0.2755(3) 0.092(2) Uani 1 1 d . . .
O2 O 1.0444(7) 0.5342(3) 0.2050(4) 0.122(4) Uani 1 1 d . . .
C51 C 0.7911(12) 0.5602(6) 0.3012(5) 0.109(4) Uani 1 1 d . . .
H51A H 0.8117 0.5882 0.3333 0.164 Uiso 1 1 calc R . .
H51B H 0.7464 0.5252 0.3163 0.164 Uiso 1 1 calc R . .
H51C H 0.7468 0.5835 0.2724 0.164 Uiso 1 1 calc R . .
C52 C 1.1506(7) 0.5103(4) 0.1724(4) 0.056(2) Uani 1 1 d . . .
H52A H 1.2087 0.5429 0.1729 0.084 Uiso 1 1 calc R . .
H52B H 1.1309 0.5003 0.1319 0.084 Uiso 1 1 calc R . .
H52C H 1.1792 0.4725 0.1917 0.084 Uiso 1 1 calc R . .
C53 C 0.9738(9) 0.5774(5) 0.2865(5) 0.086(3) Uani 1 1 d . . .
H53A H 0.9855 0.5822 0.3289 0.104 Uiso 1 1 calc R . .
H53B H 0.9592 0.6192 0.2694 0.104 Uiso 1 1 calc R . .
C54 C 1.0869(10) 0.5441(5) 0.2552(5) 0.093(4) Uani 1 1 d . . .
H54A H 1.1518 0.5731 0.2535 0.111 Uiso 1 1 calc R . .
H54B H 1.1092 0.5047 0.2749 0.111 Uiso 1 1 calc R . .
O3 O 0.534(2) 0.7423(8) -0.0241(7) 0.135(7) Uani 0.50 1 d PU . .
C61 C 0.574(3) 0.7684(11) 0.0283(9) 0.109(7) Uani 0.50 1 d PDU . .
H61A H 0.5453 0.8117 0.0325 0.131 Uiso 0.50 1 calc PR . .
H61B H 0.5468 0.7434 0.0617 0.131 Uiso 0.50 1 calc PR . .
C62 C 0.412(4) 0.7406(12) -0.0224(14) 0.147(8) Uani 0.50 1 d PDU . .
H62A H 0.3962 0.7228 0.0166 0.177 Uiso 0.50 1 calc PR . .
H62B H 0.3915 0.7855 -0.0192 0.177 Uiso 0.50 1 calc PR . .
C63 C 0.683(3) 0.7690(11) 0.0280(10) 0.119(8) Uani 0.50 1 d PDU . .
H63A H 0.7102 0.7838 0.0658 0.179 Uiso 0.50 1 calc PR . .
H63B H 0.7094 0.7972 -0.0028 0.179 Uiso 0.50 1 calc PR . .
H63C H 0.7108 0.7265 0.0207 0.179 Uiso 0.50 1 calc PR . .
C64 C 0.331(4) 0.7179(12) -0.0539(14) 0.178(10) Uani 0.50 1 d PDU . .
H64A H 0.2625 0.7426 -0.0476 0.267 Uiso 0.50 1 calc PR . .
H64B H 0.3171 0.6742 -0.0427 0.267 Uiso 0.50 1 calc PR . .
H64C H 0.3520 0.7197 -0.0952 0.267 Uiso 0.50 1 calc PR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
Li1 Br1 Sc1 76.9(3) . . ?
N1 Sc1 P3 127.43(14) . . ?
N1 Sc1 Br1 131.01(14) . . ?
P3 Sc1 Br1 101.42(6) . . ?
N1 Sc1 P2 72.62(13) . . ?
P3 Sc1 P2 104.63(6) . . ?
Br1 Sc1 P2 93.79(5) . . ?
N1 Sc1 P1 72.18(13) . . ?
P3 Sc1 P1 117.90(7) . . ?
Br1 Sc1 P1 89.56(5) . . ?
P2 Sc1 P1 135.74(6) . . ?
C14 N1 C13 116.7(5) . . ?
C14 N1 Sc1 128.7(4) . . ?
C13 N1 Sc1 114.6(3) . . ?
C7 P1 C4 106.9(3) . . ?
C7 P1 C1 105.3(3) . . ?
C4 P1 C1 103.0(4) . . ?
C7 P1 Sc1 92.40(19) . . ?
C4 P1 Sc1 128.2(3) . . ?
C1 P1 Sc1 117.7(3) . . ?
C20 P2 C21 106.1(3) . . ?
C20 P2 C24 103.7(3) . . ?
C21 P2 C24 105.2(3) . . ?
C20 P2 Sc1 99.4(2) . . ?
C21 P2 Sc1 127.0(2) . . ?
C24 P2 Sc1 112.7(2) . . ?
C3 C1 C2 109.4(7) . . ?
C3 C1 P1 112.2(5) . . ?
C2 C1 P1 114.6(6) . . ?
C3 C1 H1 106.7 . . ?
C2 C1 H1 106.7 . . ?
P1 C1 H1 106.7 . . ?
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 . . ?
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 . . ?
C5 C4 C6 112.7(7) . . ?
C5 C4 P1 109.8(5) . . ?
C6 C4 P1 109.7(6) . . ?
C5 C4 H4 108.2 . . ?
C6 C4 H4 108.2 . . ?
P1 C4 H4 108.2 . . ?
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 . . ?
C8 C7 C13 118.3(5) . . ?
C8 C7 P1 125.7(4) . . ?
C13 C7 P1 115.6(4) . . ?
C7 C8 C9 124.0(5) . . ?
C7 C8 H8 118.0 . . ?
C9 C8 H8 118.0 . . ?
C11 C9 C8 115.2(6) . . ?
C11 C9 C10 122.4(6) . . ?
C8 C9 C10 122.3(6) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C9 122.7(6) . . ?
C12 C11 H11 118.7 . . ?
C9 C11 H11 118.7 . . ?
C11 C12 C13 121.1(5) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C12 C13 C7 118.5(5) . . ?
C12 C13 N1 122.6(5) . . ?
C7 C13 N1 118.9(5) . . ?
C15 C14 C20 116.7(5) . . ?
C15 C14 N1 124.3(5) . . ?
C20 C14 N1 118.9(5) . . ?
C16 C15 C14 121.1(6) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 122.1(6) . . ?
C15 C16 H16 118.9 . . ?
C17 C16 H16 118.9 . . ?
C19 C17 C16 116.7(5) . . ?
C19 C17 C18 122.8(6) . . ?
C16 C17 C18 120.5(5) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 C20 122.1(6) . . ?
C17 C19 H19 118.9 . . ?
C20 C19 H19 118.9 . . ?
C19 C20 C14 121.2(5) . . ?
C19 C20 P2 123.0(5) . . ?
C14 C20 P2 115.7(4) . . ?
C23 C21 C22 112.4(6) . . ?
C23 C21 P2 111.5(5) . . ?
C22 C21 P2 109.5(5) . . ?
C23 C21 H21 107.7 . . ?
C22 C21 H21 107.7 . . ?
P2 C21 H21 107.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C26 C24 C25 111.7(6) . . ?
C26 C24 P2 114.7(5) . . ?
C25 C24 P2 108.7(4) . . ?
C26 C24 H24 107.2 . . ?
C25 C24 H24 107.2 . . ?
P2 C24 H24 107.2 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C27 P3 Sc1 155.2(2) . . ?
C27 P3 Li1 121.6(3) . . ?
Sc1 P3 Li1 82.5(3) . . ?
C32 C27 C28 116.8(5) . . ?
C32 C27 P3 121.3(4) . . ?
C28 C27 P3 121.9(5) . . ?
C29 C28 C27 120.5(6) . . ?
C29 C28 C33 117.1(6) . . ?
C27 C28 C33 122.4(5) . . ?
C30 C29 C28 122.0(6) . . ?
C30 C29 H29 119.0 . . ?
C28 C29 H29 119.0 . . ?
C31 C30 C29 117.7(6) . . ?
C31 C30 H30 121.1 . . ?
C29 C30 H30 121.1 . . ?
C30 C31 C32 122.8(7) . . ?
C30 C31 H31 118.6 . . ?
C32 C31 H31 118.6 . . ?
C31 C32 C27 120.2(6) . . ?
C31 C32 C42 115.8(6) . . ?
C27 C32 C42 124.0(5) . . ?
C34 C33 C38 119.2(6) . . ?
C34 C33 C28 119.9(6) . . ?
C38 C33 C28 120.6(6) . . ?
C33 C34 C35 119.4(6) . . ?
C33 C34 C39 120.1(6) . . ?
C35 C34 C39 120.4(6) . . ?
C36 C35 C34 121.6(6) . . ?
C36 C35 H35 119.2 . . ?
C34 C35 H35 119.2 . . ?
C35 C36 C37 118.6(7) . . ?
C35 C36 C40 120.7(7) . . ?
C37 C36 C40 120.7(8) . . ?
C38 C37 C36 121.6(7) . . ?
C38 C37 H37 119.2 . . ?
C36 C37 H37 119.2 . . ?
C37 C38 C33 119.5(6) . . ?
C37 C38 C41 121.3(6) . . ?
C33 C38 C41 119.2(6) . . ?
C34 C39 H39A 109.5 . . ?
C34 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C34 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C36 C40 H40A 109.5 . . ?
C36 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C36 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C47 C42 C43 118.9(6) . . ?
C47 C42 C32 118.9(5) . . ?
C43 C42 C32 121.7(5) . . ?
C44 C43 C42 119.4(6) . . ?
C44 C43 C48 121.3(5) . . ?
C42 C43 C48 119.3(6) . . ?
C43 C44 C45 122.2(6) . . ?
C43 C44 H44 118.9 . . ?
C45 C44 H44 118.9 . . ?
C46 C45 C44 117.5(6) . . ?
C46 C45 C49 121.7(6) . . ?
C44 C45 C49 120.8(6) . . ?
C45 C46 C47 123.0(6) . . ?
C45 C46 H46 118.5 . . ?
C47 C46 H46 118.5 . . ?
C46 C47 C42 118.9(6) . . ?
C46 C47 C50 120.6(6) . . ?
C42 C47 C50 120.5(6) . . ?
C43 C48 H48A 109.5 . . ?
C43 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C43 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C45 C49 H49A 109.5 . . ?
C45 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C45 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C47 C50 H50A 109.5 . . ?
C47 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C47 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O2 Li1 O1 76.4(6) . . ?
O2 Li1 P3 154.2(7) . . ?
O1 Li1 P3 115.6(6) . . ?
O2 Li1 Br1 99.5(5) . . ?
O1 Li1 Br1 104.6(5) . . ?
P3 Li1 Br1 99.1(4) . . ?
O2 Li1 C54 24.1(4) . . ?
O1 Li1 C54 58.1(5) . . ?
P3 Li1 C54 171.1(6) . . ?
Br1 Li1 C54 88.9(4) . . ?
C51 O1 C53 109.6(9) . . ?
C51 O1 Li1 130.3(9) . . ?
C53 O1 Li1 114.2(7) . . ?
C54 O2 C52 99.7(8) . . ?
C54 O2 Li1 116.9(9) . . ?
C52 O2 Li1 119.2(7) . . ?
O1 C51 H51A 109.5 . . ?
O1 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
O1 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O2 C52 H52A 109.5 . . ?
O2 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
O2 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O1 C53 C54 105.8(7) . . ?
O1 C53 H53A 110.6 . . ?
C54 C53 H53A 110.6 . . ?
O1 C53 H53B 110.6 . . ?
C54 C53 H53B 110.6 . . ?
H53A C53 H53B 108.7 . . ?
O2 C54 C53 97.9(9) . . ?
O2 C54 Li1 39.0(6) . . ?
C53 C54 Li1 76.2(6) . . ?
O2 C54 H54A 112.2 . . ?
C53 C54 H54A 112.2 . . ?
Li1 C54 H54A 150.8 . . ?
O2 C54 H54B 112.2 . . ?
C53 C54 H54B 112.2 . . ?
Li1 C54 H54B 91.0 . . ?
H54A C54 H54B 109.8 . . ?
C61 O3 C62 109(2) . . ?
C63 C61 O3 110(2) . . ?
C63 C61 H61A 109.8 . . ?
O3 C61 H61A 109.8 . . ?
C63 C61 H61B 109.8 . . ?
O3 C61 H61B 109.8 . . ?
H61A C61 H61B 108.2 . . ?
C64 C62 O3 137(4) . . ?
C64 C62 H62A 102.8 . . ?
O3 C62 H62A 102.8 . . ?
C64 C62 H62B 102.8 . . ?
O3 C62 H62B 102.8 . . ?
H62A C62 H62B 105.0 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
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
Br1 Li1 2.563(11) . ?
Br1 Sc1 2.6032(13) . ?
Sc1 N1 2.155(5) . ?
Sc1 P3 2.3732(18) . ?
Sc1 P2 2.6934(19) . ?
Sc1 P1 2.7204(19) . ?
N1 C14 1.408(7) . ?
N1 C13 1.426(8) . ?
P1 C7 1.809(6) . ?
P1 C4 1.832(7) . ?
P1 C1 1.863(7) . ?
P2 C20 1.821(6) . ?
P2 C21 1.850(6) . ?
P2 C24 1.852(6) . ?
C1 C3 1.445(12) . ?
C1 C2 1.514(11) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.434(10) . ?
C4 C6 1.516(11) . ?
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 1.388(9) . ?
C7 C13 1.410(8) . ?
C8 C9 1.397(9) . ?
C8 H8 0.9500 . ?
C9 C11 1.390(9) . ?
C9 C10 1.490(9) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.375(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.384(8) . ?
C12 H12 0.9500 . ?
C14 C15 1.401(8) . ?
C14 C20 1.402(8) . ?
C15 C16 1.386(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.394(9) . ?
C16 H16 0.9500 . ?
C17 C19 1.382(9) . ?
C17 C18 1.524(9) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.388(8) . ?
C19 H19 0.9500 . ?
C21 C23 1.519(10) . ?
C21 C22 1.528(9) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C26 1.510(9) . ?
C24 C25 1.534(9) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
P3 C27 1.822(6) . ?
P3 Li1 2.499(12) . ?
C27 C32 1.417(9) . ?
C27 C28 1.428(9) . ?
C28 C29 1.390(9) . ?
C28 C33 1.487(9) . ?
C29 C30 1.380(10) . ?
C29 H29 0.9500 . ?
C30 C31 1.379(9) . ?
C30 H30 0.9500 . ?
C31 C32 1.386(9) . ?
C31 H31 0.9500 . ?
C32 C42 1.480(9) . ?
C33 C34 1.394(9) . ?
C33 C38 1.416(9) . ?
C34 C35 1.404(10) . ?
C34 C39 1.494(10) . ?
C35 C36 1.370(11) . ?
C35 H35 0.9500 . ?
C36 C37 1.397(10) . ?
C36 C40 1.508(11) . ?
C37 C38 1.377(10) . ?
C37 H37 0.9500 . ?
C38 C41 1.509(9) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C47 1.408(9) . ?
C42 C43 1.411(8) . ?
C43 C44 1.380(8) . ?
C43 C48 1.494(9) . ?
C44 C45 1.383(9) . ?
C44 H44 0.9500 . ?
C45 C46 1.375(9) . ?
C45 C49 1.516(9) . ?
C46 C47 1.380(9) . ?
C46 H46 0.9500 . ?
C47 C50 1.482(10) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
Li1 O2 1.969(13) . ?
Li1 O1 2.047(15) . ?
Li1 C54 2.789(15) . ?
O1 C51 1.360(12) . ?
O1 C53 1.368(11) . ?
O2 C54 1.275(12) . ?
O2 C52 1.555(12) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.680(16) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
O3 C61 1.41(3) . ?
O3 C62 1.46(4) . ?
C61 C63 1.29(3) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C64 1.30(3) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
