#------------------------------------------------------------------------------
#$Date: 2016-03-21 13:06:47 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178691 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/02/4080202.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_4080202
loop_
_publ_author_name
'Kratsch, Jochen'
'Kuzdrowska, Magdalena'
'Schmid, Matthias'
'Kazeminejad, Neda'
'Kaub, Christoph'
'Oña-Burgos, Pascual'
'Guillaume, Sophie M.'
'Roesky, Peter W.'
_publ_section_title
;
 Chiral Rare Earth Borohydride Complexes Supported by Amidinate Ligands:
 Synthesis, Structure, and Catalytic Activity in the Ring-Opening
 Polymerization ofrac-Lactide
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1230
_journal_paper_doi               10.1021/om301011v
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C31 H47 B2 N2 O2 Yb'
_chemical_formula_sum            'C31 H47 B2 N2 O2 Yb'
_chemical_formula_weight         674.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 118.16(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.256(3)
_cell_length_b                   12.600(3)
_cell_length_c                   10.874(2)
_cell_measurement_reflns_used    17930
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      2.12
_cell_volume                     1601.3(8)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Diamond 3.2g'
_computing_publication_material  'WinGX, Microsoft Word'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'area detector'
_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  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9473
_diffrn_reflns_theta_full        29.15
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    2.948
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.6445
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.183
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.018(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         4318
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0352P)²+1.2086P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0590
_reflns_number_gt                4318
_reflns_number_total             4318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301011v_si_002.cif
_cod_data_source_block           5
_cod_original_cell_volume        1601.2(6)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4080202
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-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
C1 C 0.5000 0.3028(3) 0.5000 0.0265(7) Uani 1 2 d S
C2 C 0.5000 0.4222(3) 0.5000 0.0290(8) Uani 1 2 d S
C3 C 0.3972(3) 0.4777(3) 0.4413(4) 0.0378(7) Uani 1 1 d .
H20 H 0.3267 0.4402 0.4016 0.045 Uiso 1 1 calc R
C4 C 0.3974(4) 0.5860(9) 0.4407(4) 0.0512(9) Uani 1 1 d .
H21 H 0.3266 0.6232 0.3994 0.061 Uiso 1 1 calc R
C5 C 0.5000 0.6434(4) 0.5000 0.0552(16) Uani 1 2 d S
H22 H 0.5000 0.7188 0.5000 0.066 Uiso 1 2 calc SR
C6 C 0.4854(3) 0.2969(2) 0.7156(4) 0.0312(6) Uani 1 1 d .
H2 H 0.4770 0.3750 0.6967 0.037 Uiso 1 1 calc R
C7 C 0.3812(3) 0.2598(3) 0.7283(4) 0.0399(7) Uani 1 1 d .
H3A H 0.3118 0.2724 0.6399 0.060 Uiso 1 1 calc R
H3B H 0.3766 0.2994 0.8030 0.060 Uiso 1 1 calc R
H3C H 0.3883 0.1839 0.7501 0.060 Uiso 1 1 calc R
C8 C 0.5961(3) 0.2795(3) 0.8504(4) 0.0369(6) Uani 1 1 d .
C9 C 0.6726(5) 0.3644(5) 0.9048(6) 0.0521(11) Uani 1 1 d .
H4 H 0.6549 0.4316 0.8597 0.062 Uiso 1 1 calc R
C10 C 0.7771(5) 0.3482(7) 1.0287(6) 0.0703(16) Uani 1 1 d .
H10 H 0.8304 0.4048 1.0662 0.084 Uiso 1 1 calc R
C11 C 0.8018(6) 0.2523(8) 1.0945(7) 0.074(2) Uani 1 1 d .
H11 H 0.8720 0.2426 1.1775 0.088 Uiso 1 1 calc R
C12 C 0.7257(5) 0.1695(5) 1.0414(5) 0.0659(15) Uani 1 1 d .
H12 H 0.7436 0.1030 1.0881 0.079 Uiso 1 1 calc R
C13 C 0.6222(4) 0.1825(4) 0.9193(4) 0.0486(9) Uani 1 1 d .
H6 H 0.5698 0.1250 0.8835 0.058 Uiso 1 1 calc R
C14 C 0.2348(4) 0.1964(4) 0.3127(5) 0.0436(9) Uani 1 1 d .
H9A H 0.2643 0.2519 0.2737 0.052 Uiso 1 1 calc R
H9B H 0.2355 0.2245 0.3982 0.052 Uiso 1 1 calc R
C15 C 0.1166(5) 0.1651(6) 0.2086(7) 0.0681(15) Uani 1 1 d .
H15A H 0.0639 0.1718 0.2492 0.082 Uiso 1 1 calc R
H15B H 0.0884 0.2110 0.1250 0.082 Uiso 1 1 calc R
C16 C 0.1231(6) 0.0530(5) 0.1711(8) 0.077(2) Uani 1 1 d .
H16A H 0.0550 0.0127 0.1594 0.092 Uiso 1 1 calc R
H16B H 0.1283 0.0488 0.0833 0.092 Uiso 1 1 calc R
C17 C 0.2279(5) 0.0111(5) 0.2892(7) 0.0533(13) Uani 1 1 d .
H13A H 0.2106 -0.0192 0.3612 0.064 Uiso 1 1 calc R
H13B H 0.2625 -0.0450 0.2573 0.064 Uiso 1 1 calc R
B B 0.5532(5) -0.0416(4) 0.3554(6) 0.0494(11) Uani 1 1 d .
N N 0.4891(2) 0.2450(2) 0.5962(3) 0.0305(5) Uani 1 1 d .
O O 0.3048(2) 0.1011(2) 0.3447(3) 0.0397(8) Uani 1 1 d .
Yb Yb 0.5000 0.0835 0.5000 0.02928(5) Uani 1 2 d S
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'
B B 0.0013 0.0007 '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'
Yb Yb -0.3850 5.5486 '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
N C1 N 114.0(3) 2_656 .
N C1 C2 123.01(17) 2_656 .
N C1 C2 123.01(17) . .
N C1 Yb 56.99(17) 2_656 .
N C1 Yb 56.99(17) . .
C2 C1 Yb 180.0 . .
C3 C2 C3 119.6(4) 2_656 .
C3 C2 C1 120.2(2) 2_656 .
C3 C2 C1 120.2(2) . .
C4 C3 C2 120.1(4) . .
C3 C4 C5 121.1(5) . .
C4 C5 C4 117.9(8) . 2_656
N C6 C8 111.5(3) . .
N C6 C7 110.6(3) . .
C8 C6 C7 111.8(3) . .
C13 C8 C9 119.9(4) . .
C13 C8 C6 121.8(3) . .
C9 C8 C6 118.3(4) . .
C8 C9 C10 118.6(6) . .
C11 C10 C9 120.7(5) . .
C10 C11 C12 120.3(5) . .
C11 C12 C13 120.5(6) . .
C8 C13 C12 119.9(5) . .
O C14 C15 106.6(4) . .
C16 C15 C14 106.5(5) . .
C17 C16 C15 104.7(5) . .
O C17 C16 105.7(4) . .
C1 N C6 120.5(2) . .
C1 N Yb 94.13(19) . .
C6 N Yb 145.10(19) . .
C17 O C14 107.6(4) . .
C17 O Yb 123.1(3) . .
C14 O Yb 127.8(3) . .
N Yb N 57.77(13) . 2_656
N Yb O 82.82(10) . 2_656
N Yb O 87.68(10) 2_656 2_656
N Yb O 87.68(10) . .
N Yb O 82.82(10) 2_656 .
O Yb O 169.16(14) 2_656 .
N Yb B 99.74(14) . 2_656
N Yb B 155.96(15) 2_656 2_656
O Yb B 98.45(15) 2_656 2_656
O Yb B 88.27(14) . 2_656
N Yb B 155.96(15) . .
N Yb B 99.74(14) 2_656 .
O Yb B 88.27(14) 2_656 .
O Yb B 98.45(15) . .
B Yb B 103.6(3) 2_656 .
N Yb C1 28.89(6) . .
N Yb C1 28.89(6) 2_656 .
O Yb C1 84.58(7) 2_656 .
O Yb C1 84.58(7) . .
B Yb C1 128.18(13) 2_656 .
B Yb C1 128.18(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N 1.338(3) 2_656
C1 N 1.338(3) .
C1 C2 1.504(5) .
C1 Yb 2.763(4) .
C2 C3 1.390(4) 2_656
C2 C3 1.390(4) .
C3 C4 1.365(12) .
C4 C5 1.400(8) .
C5 C4 1.400(9) 2_656
C6 N 1.474(4) .
C6 C8 1.523(5) .
C6 C7 1.525(5) .
C8 C13 1.390(6) .
C8 C9 1.398(7) .
C9 C10 1.419(10) .
C10 C11 1.364(12) .
C11 C12 1.374(12) .
C12 C13 1.397(7) .
C14 O 1.456(6) .
C14 C15 1.490(7) .
C15 C16 1.484(10) .
C16 C17 1.475(8) .
C17 O 1.452(6) .
B Yb 2.550(5) .
N Yb 2.323(3) .
O Yb 2.340(3) .
Yb N 2.323(3) 2_656
Yb O 2.340(3) 2_656
Yb B 2.550(5) 2_656
