#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:41:20 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179257 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/77/4317702.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_4317702
loop_
_publ_author_name
'Gerd W. Rabe'
'Christian D. Bérubé'
'Glenn P. A. Yap'
'Kin-Chung Lam'
'Thomas E. Concolino'
'Arnold L. Rheingold'
_publ_section_title
;
 Synthesis and Structural Characterization of 2,6-Dimesitylphenyl
 Complexes of Scandium, Ytterbium, and Yttrium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1446
_journal_page_last               1453
_journal_paper_doi               10.1021/ic0109492
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C32 H41 Cl2 O2 Sc'
_chemical_formula_weight         573.51
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.178(3)
_cell_length_b                   15.468(5)
_cell_length_c                   20.132(5)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.47
_cell_volume                     3101.9(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.880
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17881
_diffrn_reflns_theta_full        28.61
_diffrn_reflns_theta_max         28.61
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.928076
_exptl_absorpt_correction_T_min  0.757406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing,R., Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0036(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         6989
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0662P)²+4.9346P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1786
_reflns_number_gt                4727
_reflns_number_total             6989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0109492_1.cif
_cod_data_source_block           gr008
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3102.0(17)
_cod_database_code               4317702
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Sc Sc 0.48490(6) 0.84139(4) 0.83354(3) 0.03846(18) Uani 1 1 d . . .
Cl1 Cl 0.36603(10) 0.71373(6) 0.78390(5) 0.0526(2) Uani 1 1 d . A .
Cl2 Cl 0.57694(9) 0.97746(6) 0.87853(5) 0.0522(2) Uani 1 1 d . A .
C1 C 0.7125(3) 0.8119(2) 1.02667(16) 0.0402(7) Uani 1 1 d . . .
C2 C 0.6614(3) 0.8221(2) 1.08544(16) 0.0444(8) Uani 1 1 d . . .
H2A H 0.6952 0.8665 1.1161 0.053 Uiso 1 1 calc R . .
C3 C 0.5613(3) 0.7679(2) 1.09976(16) 0.0443(8) Uani 1 1 d . . .
C4 C 0.5137(3) 0.7026(2) 1.05421(17) 0.0445(8) Uani 1 1 d . . .
H4A H 0.4458 0.6660 1.0633 0.053 Uiso 1 1 calc R . .
C5 C 0.5633(3) 0.6893(2) 0.99488(16) 0.0409(7) Uani 1 1 d . . .
C6 C 0.6633(3) 0.7448(2) 0.98091(15) 0.0371(7) Uani 1 1 d . A .
C7 C 0.8227(4) 0.8713(3) 1.01407(18) 0.0488(8) Uani 1 1 d . . .
H7A H 0.8435 0.9132 1.0505 0.073 Uiso 1 1 calc R . .
H7B H 0.7932 0.9011 0.9712 0.073 Uiso 1 1 calc R . .
H7C H 0.9023 0.8375 1.0124 0.073 Uiso 1 1 calc R . .
C8 C 0.5067(4) 0.7813(3) 1.16347(18) 0.0555(10) Uani 1 1 d . . .
H8A H 0.5802 0.7811 1.2027 0.083 Uiso 1 1 calc R . .
H8B H 0.4445 0.7352 1.1677 0.083 Uiso 1 1 calc R . .
H8C H 0.4604 0.8364 1.1608 0.083 Uiso 1 1 calc R . .
C9 C 0.5142(4) 0.6132(3) 0.94975(18) 0.0528(9) Uani 1 1 d . . .
H9A H 0.5552 0.6143 0.9103 0.079 Uiso 1 1 calc R . .
H9B H 0.4173 0.6163 0.9352 0.079 Uiso 1 1 calc R . .
H9C H 0.5384 0.5599 0.9747 0.079 Uiso 1 1 calc R . .
C10 C 0.7277(3) 0.7287(2) 0.92099(15) 0.0377(7) Uani 1 1 d . . .
C11 C 0.8381(4) 0.6735(2) 0.93220(17) 0.0455(8) Uani 1 1 d . A .
H11A H 0.8668 0.6480 0.9751 0.055 Uiso 1 1 calc R . .
C12 C 0.9059(4) 0.6558(3) 0.88076(18) 0.0528(9) Uani 1 1 d . . .
H12A H 0.9784 0.6170 0.8881 0.063 Uiso 1 1 calc R A .
C13 C 0.8655(4) 0.6961(2) 0.81836(18) 0.0472(8) Uani 1 1 d . A .
H13A H 0.9125 0.6855 0.7836 0.057 Uiso 1 1 calc R . .
C14 C 0.7560(3) 0.7523(2) 0.80669(15) 0.0376(7) Uani 1 1 d . . .
C15 C 0.6804(3) 0.7691(2) 0.85747(15) 0.0369(7) Uani 1 1 d . A .
C16 C 0.6554(4) 0.7545(2) 0.68077(17) 0.0446(8) Uani 1 1 d . . .
C17 C 0.6355(4) 0.7974(2) 0.61813(17) 0.0487(8) Uani 1 1 d . A .
H17A H 0.5893 0.7686 0.5791 0.058 Uiso 1 1 calc R . .
C18 C 0.6812(4) 0.8807(2) 0.61156(17) 0.0461(8) Uani 1 1 d . . .
C19 C 0.7509(4) 0.9216(2) 0.66946(18) 0.0461(8) Uani 1 1 d . A .
H19A H 0.7840 0.9777 0.6658 0.055 Uiso 1 1 calc R . .
C20 C 0.7732(3) 0.8818(2) 0.73310(16) 0.0413(7) Uani 1 1 d . . .
C21 C 0.7241(3) 0.7976(2) 0.73908(16) 0.0380(7) Uani 1 1 d . A .
C22 C 0.6103(5) 0.6621(3) 0.6832(2) 0.0621(11) Uani 1 1 d . A .
H22A H 0.6307 0.6418 0.7298 0.093 Uiso 1 1 calc R . .
H22B H 0.6569 0.6264 0.6558 0.093 Uiso 1 1 calc R . .
H22C H 0.5143 0.6585 0.6656 0.093 Uiso 1 1 calc R . .
C23 C 0.6608(4) 0.9243(3) 0.54309(19) 0.0605(10) Uani 1 1 d . A .
H23A H 0.6955 0.9829 0.5487 0.091 Uiso 1 1 calc R . .
H23B H 0.5657 0.9259 0.5228 0.091 Uiso 1 1 calc R . .
H23C H 0.7080 0.8923 0.5138 0.091 Uiso 1 1 calc R . .
C24 C 0.8590(4) 0.9266(3) 0.79340(19) 0.0545(9) Uani 1 1 d . A .
H24A H 0.8784 0.9850 0.7808 0.082 Uiso 1 1 calc R . .
H24B H 0.9424 0.8951 0.8077 0.082 Uiso 1 1 calc R . .
H24C H 0.8113 0.9285 0.8304 0.082 Uiso 1 1 calc R . .
O1 O 0.3433(2) 0.84970(17) 0.89997(12) 0.0493(6) Uani 1 1 d D A .
C25 C 0.2117(5) 0.8081(5) 0.8876(3) 0.104(2) Uani 1 1 d D . .
H25A H 0.2205 0.7457 0.8959 0.124 Uiso 1 1 calc R A .
H25B H 0.1635 0.8179 0.8409 0.124 Uiso 1 1 calc R . .
C26 C 0.1395(5) 0.8506(4) 0.9376(3) 0.0928(19) Uani 1 1 d D A .
H26A H 0.0948 0.9040 0.9187 0.111 Uiso 1 1 calc R . .
H26B H 0.0726 0.8116 0.9500 0.111 Uiso 1 1 calc R . .
C27 C 0.2467(4) 0.8689(3) 0.9958(2) 0.0681(12) Uani 1 1 d D . .
H27A H 0.2714 0.8170 1.0234 0.082 Uiso 1 1 calc R A .
H27B H 0.2201 0.9144 1.0243 0.082 Uiso 1 1 calc R . .
C28 C 0.3611(4) 0.8987(3) 0.96418(18) 0.0543(9) Uani 1 1 d D A .
H28A H 0.3558 0.9610 0.9555 0.065 Uiso 1 1 calc R . .
H28B H 0.4478 0.8853 0.9937 0.065 Uiso 1 1 calc R . .
O2 O 0.3935(3) 0.90916(16) 0.74137(12) 0.0525(6) Uani 0.70 1 d PD A 1
C29 C 0.3215(17) 0.8697(7) 0.6787(5) 0.149(7) Uani 0.70 1 d PD A 1
H29A H 0.2308 0.8521 0.6824 0.179 Uiso 0.70 1 calc PR A 1
H29B H 0.3699 0.8194 0.6662 0.179 Uiso 0.70 1 calc PR A 1
C30 C 0.3177(12) 0.9455(7) 0.6264(5) 0.092(3) Uani 0.70 1 d PD A 1
H30A H 0.4025 0.9497 0.6107 0.110 Uiso 0.70 1 calc PR A 1
H30B H 0.2439 0.9380 0.5870 0.110 Uiso 0.70 1 calc PR A 1
C31 C 0.2980(7) 1.0160(4) 0.6633(3) 0.0692(18) Uani 0.70 1 d PD A 1
H31A H 0.2070 1.0171 0.6724 0.083 Uiso 0.70 1 calc PR A 1
H31B H 0.3145 1.0698 0.6406 0.083 Uiso 0.70 1 calc PR A 1
C32 C 0.4029(9) 1.0015(5) 0.7280(4) 0.078(2) Uani 0.70 1 d PD A 1
H32A H 0.4928 1.0167 0.7213 0.094 Uiso 0.70 1 calc PR A 1
H32B H 0.3827 1.0360 0.7655 0.094 Uiso 0.70 1 calc PR A 1
O2' O 0.3935(3) 0.90916(16) 0.74137(12) 0.0525(6) Uani 0.30 1 d PD A 2
C29' C 0.3506(14) 0.8765(10) 0.6736(5) 0.042(4) Uani 0.30 1 d PD A 2
H29C H 0.3008 0.8223 0.6736 0.050 Uiso 0.30 1 calc PR A 2
H29D H 0.4275 0.8667 0.6522 0.050 Uiso 0.30 1 calc PR A 2
C30' C 0.259(3) 0.9487(10) 0.6368(8) 0.21(3) Uani 0.30 1 d PD A 2
H30C H 0.3128 0.9953 0.6227 0.256 Uiso 0.30 1 calc PR A 2
H30D H 0.1978 0.9259 0.5967 0.256 Uiso 0.30 1 calc PR A 2
C31' C 0.1893(15) 0.9780(11) 0.6842(10) 0.084(6) Uani 0.30 1 d PD A 2
H31C H 0.1206 0.9366 0.6912 0.101 Uiso 0.30 1 calc PR A 2
H31D H 0.1473 1.0343 0.6714 0.101 Uiso 0.30 1 calc PR A 2
C32' C 0.304(3) 0.9851(14) 0.7471(10) 0.142(13) Uani 0.30 1 d PD A 2
H32C H 0.3527 1.0396 0.7469 0.171 Uiso 0.30 1 calc PR A 2
H32D H 0.2690 0.9816 0.7889 0.171 Uiso 0.30 1 calc PR A 2
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.2519 0.3716 '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
O1 Sc O2 106.11(10) . . ?
O1 Sc C15 124.79(11) . . ?
O2 Sc C15 129.02(11) . . ?
O1 Sc Cl2 88.43(8) . . ?
O2 Sc Cl2 87.97(8) . . ?
C15 Sc Cl2 95.48(9) . . ?
O1 Sc Cl1 87.93(8) . . ?
O2 Sc Cl1 87.18(8) . . ?
C15 Sc Cl1 91.61(9) . . ?
Cl2 Sc Cl1 172.89(4) . . ?
C2 C1 C6 119.5(3) . . ?
C2 C1 C7 119.5(3) . . ?
C6 C1 C7 120.9(3) . . ?
C3 C2 C1 121.5(3) . . ?
C4 C3 C2 118.2(3) . . ?
C4 C3 C8 121.5(3) . . ?
C2 C3 C8 120.2(3) . . ?
C3 C4 C5 122.2(3) . . ?
C6 C5 C4 118.9(3) . . ?
C6 C5 C9 121.4(3) . . ?
C4 C5 C9 119.6(3) . . ?
C5 C6 C1 119.6(3) . . ?
C5 C6 C10 120.8(3) . . ?
C1 C6 C10 119.4(3) . . ?
C11 C10 C15 122.1(3) . . ?
C11 C10 C6 116.2(3) . . ?
C15 C10 C6 121.8(3) . . ?
C12 C11 C10 120.6(3) . . ?
C11 C12 C13 119.2(3) . . ?
C12 C13 C14 120.7(3) . . ?
C13 C14 C15 121.6(3) . . ?
C13 C14 C21 117.3(3) . . ?
C15 C14 C21 121.0(3) . . ?
C10 C15 C14 115.7(3) . . ?
C10 C15 Sc 122.4(2) . . ?
C14 C15 Sc 121.5(2) . . ?
C17 C16 C21 118.8(3) . . ?
C17 C16 C22 119.4(3) . . ?
C21 C16 C22 121.8(3) . . ?
C18 C17 C16 122.5(3) . . ?
C19 C18 C17 117.9(3) . . ?
C19 C18 C23 120.9(3) . . ?
C17 C18 C23 121.1(3) . . ?
C18 C19 C20 121.9(3) . . ?
C19 C20 C21 119.5(3) . . ?
C19 C20 C24 119.5(3) . . ?
C21 C20 C24 120.8(3) . . ?
C16 C21 C20 119.5(3) . . ?
C16 C21 C14 120.8(3) . . ?
C20 C21 C14 119.6(3) . . ?
C25 O1 C28 108.5(3) . . ?
C25 O1 Sc 125.0(2) . . ?
C28 O1 Sc 126.5(2) . . ?
O1 C25 C26 104.5(4) . . ?
C27 C26 C25 103.5(4) . . ?
C26 C27 C28 103.6(4) . . ?
O1 C28 C27 104.3(3) . . ?
C29 O2 C32 106.9(5) . . ?
C29 O2 Sc 126.1(4) . . ?
C32 O2 Sc 126.7(3) . . ?
O2 C29 C30 101.9(8) . . ?
C31 C30 C29 102.6(8) . . ?
C30 C31 C32 101.2(7) . . ?
O2 C32 C31 103.9(5) . . ?
C31' C30' C29' 104.6(12) . . ?
C30' C31' C32' 100.4(13) . . ?
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
Sc O1 2.162(2) . ?
Sc O2 2.168(2) . ?
Sc C15 2.247(3) . ?
Sc Cl2 2.4040(13) . ?
Sc Cl1 2.4219(13) . ?
C1 C2 1.396(4) . ?
C1 C6 1.410(5) . ?
C1 C7 1.511(5) . ?
C2 C3 1.394(5) . ?
C3 C4 1.382(5) . ?
C3 C8 1.513(4) . ?
C4 C5 1.404(4) . ?
C5 C6 1.403(5) . ?
C5 C9 1.509(5) . ?
C6 C10 1.507(4) . ?
C10 C11 1.391(5) . ?
C10 C15 1.416(4) . ?
C11 C12 1.384(5) . ?
C12 C13 1.387(5) . ?
C13 C14 1.394(5) . ?
C14 C15 1.424(4) . ?
C14 C21 1.506(4) . ?
C16 C17 1.403(5) . ?
C16 C21 1.406(5) . ?
C16 C22 1.505(5) . ?
C17 C18 1.385(5) . ?
C18 C19 1.387(5) . ?
C18 C23 1.511(5) . ?
C19 C20 1.397(5) . ?
C20 C21 1.408(5) . ?
C20 C24 1.511(5) . ?
O1 C25 1.461(5) . ?
O1 C28 1.477(4) . ?
C25 C26 1.512(6) . ?
C26 C27 1.456(6) . ?
C27 C28 1.509(5) . ?
O2 C29 1.457(9) . ?
O2 C32 1.460(7) . ?
C29 C30 1.572(11) . ?
C30 C31 1.358(11) . ?
C31 C32 1.521(8) . ?
C29' C30' 1.541(14) . ?
C30' C31' 1.379(17) . ?
C31' C32' 1.540(15) . ?
