#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:04:25 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178593 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/04/4070465.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_4070465
loop_
_publ_author_name
'Zimmermann, Melanie'
'Litlabø, Rannveig'
'Törnroos, Karl W.'
'Anwander, Reiner'
_publ_section_title
;
 “Metastable” Lu(GaMe4)3Reacts Like Masked [LuMe3]:
 Synthesis of an Unsolvated Lanthanide Dimethyl Complex
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6646
_journal_paper_doi               10.1021/om900838h
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C26 H46 B Lu N6'
_chemical_formula_sum            'C26 H46 B Lu N6'
_chemical_formula_weight         628.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   18.0766(6)
_cell_length_b                   16.7735(6)
_cell_length_c                   9.8459(4)
_cell_measurement_reflns_used    24760
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.15
_cell_measurement_theta_min      2.35
_cell_volume                     2985.35(19)
_computing_cell_refinement
;
Bruker (2008). SAINT, version 7.56A, Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_data_collection
;
Bruker (1999). SMART, version 5.054, Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_data_reduction
;
Bruker (2004). SAINT, version 6.45a, Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_molecular_graphics
;
Brandenburg, K. (2007). DIAMOND. Version 3.1. Crystal Impact GbR, Bonn, 
Germany.
;
_computing_publication_material
;
Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_structure_refinement
;
Sheldrick, G. M. (2008). Acta Crystallographica, A64, 112-122.
;
_computing_structure_solution
;     
Sheldrick, G. M. (2008). Acta Crystallographica, A64, 112-122.
;
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean '48 \um'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker-AXS SMART 2K CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0104
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            47440
_diffrn_reflns_theta_full        30.16
_diffrn_reflns_theta_max         30.16
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    3.330
_exptl_absorpt_correction_T_max  0.5855
_exptl_absorpt_correction_T_min  0.4155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS version 2008/1, G.M Sheldrick, University of 
Gẗtingen, Germany, 2008.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.435
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0176P)²+3.1117P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0461
_reflns_number_gt                4165
_reflns_number_total             4553
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om900838h_si_001.cif
_cod_data_source_block           Compound3
_cod_database_code               4070465
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
Lu1 Lu 0.120281(5) 0.7500 0.435610(9) 0.02022(3) Uani 1 2 d S
N1 N -0.02332(8) 0.67258(10) 0.31023(14) 0.0240(3) Uani 1 1 d .
N2 N 0.04499(8) 0.64685(10) 0.35534(15) 0.0236(3) Uani 1 1 d .
N3 N -0.05497(11) 0.7500 0.5216(2) 0.0208(4) Uani 1 2 d S
N4 N 0.01188(11) 0.7500 0.5905(2) 0.0221(4) Uani 1 2 d S
B1 B -0.05961(15) 0.7500 0.3654(3) 0.0231(5) Uani 1 2 d S
H1B H -0.1156(16) 0.7500 0.332(3) 0.028 Uiso 1 2 d S
C1 C 0.22969(15) 0.7500 0.5671(3) 0.0335(6) Uani 1 2 d S
H1A H 0.2728 0.7500 0.5067 0.050 Uiso 1 2 calc SR
H1C H 0.2308 0.7023 0.6245 0.050 Uiso 0.50 1 calc PR
H1D H 0.2308 0.7977 0.6245 0.050 Uiso 0.50 1 calc PR
C2 C 0.18127(14) 0.7500 0.2219(2) 0.0279(5) Uani 1 2 d S
H2A H 0.2349 0.7500 0.2361 0.042 Uiso 1 2 calc SR
H2B H 0.1670 0.7977 0.1708 0.042 Uiso 0.50 1 calc PR
H2C H 0.1670 0.7023 0.1708 0.042 Uiso 0.50 1 calc PR
C3 C -0.05370(11) 0.61525(13) 0.23126(19) 0.0319(4) Uani 1 1 d .
C4 C -0.00490(12) 0.55245(14) 0.2238(2) 0.0369(4) Uani 1 1 d .
H4A H -0.0112 0.5042 0.1745 0.044 Uiso 1 1 calc R
C5 C 0.05586(10) 0.57407(12) 0.30361(19) 0.0286(4) Uani 1 1 d .
C6 C -0.12952(12) 0.62192(17) 0.1698(3) 0.0453(6) Uani 1 1 d .
H6A H -0.1316 0.6690 0.1111 0.068 Uiso 1 1 calc R
H6B H -0.1664 0.6270 0.2424 0.068 Uiso 1 1 calc R
H6C H -0.1400 0.5741 0.1161 0.068 Uiso 1 1 calc R
C7 C 0.12263(11) 0.52422(13) 0.3406(2) 0.0340(4) Uani 1 1 d .
C8 C 0.16244(16) 0.49694(19) 0.2110(3) 0.0582(7) Uani 1 1 d .
H8A H 0.1783 0.5437 0.1590 0.087 Uiso 1 1 calc R
H8B H 0.1286 0.4648 0.1558 0.087 Uiso 1 1 calc R
H8C H 0.2058 0.4649 0.2355 0.087 Uiso 1 1 calc R
C9 C 0.09511(16) 0.45150(15) 0.4213(3) 0.0515(6) Uani 1 1 d .
H9A H 0.0695 0.4696 0.5035 0.077 Uiso 1 1 calc R
H9B H 0.1374 0.4181 0.4468 0.077 Uiso 1 1 calc R
H9C H 0.0609 0.4205 0.3650 0.077 Uiso 1 1 calc R
C10 C 0.17599(11) 0.57118(14) 0.4295(2) 0.0371(4) Uani 1 1 d .
H10A H 0.1951 0.6169 0.3784 0.056 Uiso 1 1 calc R
H10B H 0.2172 0.5367 0.4566 0.056 Uiso 1 1 calc R
H10C H 0.1500 0.5901 0.5107 0.056 Uiso 1 1 calc R
C11 C -0.11184(13) 0.7500 0.6110(3) 0.0239(5) Uani 1 2 d S
C12 C -0.08238(14) 0.7500 0.7405(3) 0.0272(5) Uani 1 2 d S
H12A H -0.1089 0.7500 0.8238 0.033 Uiso 1 2 calc SR
C13 C -0.00548(13) 0.7500 0.7242(2) 0.0245(5) Uani 1 2 d S
C14 C -0.19147(14) 0.7500 0.5691(3) 0.0302(6) Uani 1 2 d S
H14A H -0.1947 0.7500 0.4697 0.045 Uiso 1 2 calc SR
H14B H -0.2159 0.7977 0.6050 0.045 Uiso 0.50 1 calc PR
H14C H -0.2159 0.7023 0.6050 0.045 Uiso 0.50 1 calc PR
C15 C 0.05256(14) 0.7500 0.8349(3) 0.0323(6) Uani 1 2 d S
C16 C 0.10106(13) 0.67566(15) 0.8242(3) 0.0475(6) Uani 1 1 d .
H16A H 0.1276 0.6762 0.7374 0.071 Uiso 1 1 calc R
H16B H 0.0699 0.6279 0.8292 0.071 Uiso 1 1 calc R
H16C H 0.1368 0.6751 0.8990 0.071 Uiso 1 1 calc R
C18 C 0.0140(2) 0.7500 0.9733(3) 0.100(3) Uani 1 2 d S
H18A H 0.0512 0.7500 1.0456 0.150 Uiso 1 2 calc SR
H18B H -0.0170 0.7023 0.9815 0.150 Uiso 0.50 1 calc PR
H18C H -0.0170 0.7977 0.9815 0.150 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'
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'
Lu Lu -0.4720 5.8584 '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
N2 Lu1 N2 95.42(8) . 7_575
N2 Lu1 C1 132.22(4) . .
N2 Lu1 C1 132.22(4) 7_575 .
N2 Lu1 C2 88.33(5) . .
N2 Lu1 C2 88.33(5) 7_575 .
C1 Lu1 C2 95.55(9) . .
N2 Lu1 N4 75.43(5) . .
N2 Lu1 N4 75.43(5) 7_575 .
C1 Lu1 N4 108.90(8) . .
C2 Lu1 N4 155.56(8) . .
C3 N1 N2 109.01(15) . .
C3 N1 B1 128.59(16) . .
N2 N1 B1 121.76(15) . .
C5 N2 N1 107.09(15) . .
C5 N2 Lu1 135.93(12) . .
N1 N2 Lu1 113.44(11) . .
C11 N3 N4 110.13(19) . .
C11 N3 B1 127.4(2) . .
N4 N3 B1 122.43(19) . .
C13 N4 N3 105.89(19) . .
C13 N4 Lu1 141.32(16) . .
N3 N4 Lu1 112.80(14) . .
N3 B1 N1 109.04(13) . .
N3 B1 N1 109.04(13) . 7_575
N1 B1 N1 113.5(2) . 7_575
N3 B1 H1B 110.9(18) . .
N1 B1 H1B 107.2(9) . .
N1 B1 H1B 107.2(9) 7_575 .
Lu1 C1 H1A 109.5 . .
Lu1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
Lu1 C1 H1D 109.5 . .
H1A C1 H1D 109.5 . .
H1C C1 H1D 109.5 . .
Lu1 C2 H2A 109.5 . .
Lu1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
Lu1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N1 C3 C4 108.32(17) . .
N1 C3 C6 123.3(2) . .
C4 C3 C6 128.35(19) . .
C3 C4 C5 105.97(18) . .
C3 C4 H4A 127.0 . .
C5 C4 H4A 127.0 . .
N2 C5 C4 109.60(18) . .
N2 C5 C7 122.02(17) . .
C4 C5 C7 128.21(19) . .
C3 C6 H6A 109.5 . .
C3 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C3 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 C10 110.97(17) . .
C5 C7 C8 109.81(19) . .
C10 C7 C8 109.60(19) . .
C5 C7 C9 107.73(18) . .
C10 C7 C9 108.5(2) . .
C8 C7 C9 110.2(2) . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C7 C10 H10A 109.5 . .
C7 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C7 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N3 C11 C12 107.9(2) . .
N3 C11 C14 123.4(2) . .
C12 C11 C14 128.7(2) . .
C11 C12 C13 106.1(2) . .
C11 C12 H12A 127.0 . .
C13 C12 H12A 127.0 . .
N4 C13 C12 110.0(2) . .
N4 C13 C15 122.7(2) . .
C12 C13 C15 127.3(2) . .
C11 C14 H14A 109.5 . .
C11 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C11 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 C16 110.38(15) . 7_575
C13 C15 C16 110.38(15) . .
C16 C15 C16 109.4(2) 7_575 .
C13 C15 C18 109.0(2) . .
C16 C15 C18 108.84(17) 7_575 .
C16 C15 C18 108.84(17) . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 C18 H18A 109.5 . .
C15 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C15 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Lu1 N2 2.3388(15) .
Lu1 N2 2.3389(15) 7_575
Lu1 C1 2.364(3) .
Lu1 C2 2.375(2) .
Lu1 N4 2.483(2) .
N1 C3 1.353(2) .
N1 N2 1.381(2) .
N1 B1 1.553(2) .
N2 C5 1.337(2) .
N3 C11 1.353(3) .
N3 N4 1.386(3) .
N3 B1 1.541(3) .
N4 C13 1.353(3) .
B1 N1 1.553(2) 7_575
B1 H1B 1.06(3) .
C1 H1A 0.9800 .
C1 H1C 0.9800 .
C1 H1D 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C4 1.376(3) .
C3 C6 1.502(3) .
C4 C5 1.398(3) .
C4 H4A 0.9500 .
C5 C7 1.513(3) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 C10 1.522(3) .
C7 C8 1.535(3) .
C7 C9 1.538(3) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.382(3) .
C11 C14 1.497(3) .
C12 C13 1.399(3) .
C12 H12A 0.9500 .
C13 C15 1.513(3) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C16 1.528(3) 7_575
C15 C16 1.528(3) .
C15 C18 1.531(4) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
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_4
C3 N1 N2 C5 0.03(19) . .
B1 N1 N2 C5 171.55(16) . .
C3 N1 N2 Lu1 162.33(12) . .
B1 N1 N2 Lu1 -26.15(19) . .
N2 Lu1 N2 C5 144.57(15) 7_575 .
C1 Lu1 N2 C5 -39.6(2) . .
C2 Lu1 N2 C5 56.41(18) . .
N4 Lu1 N2 C5 -142.03(18) . .
N2 Lu1 N2 N1 -10.73(13) 7_575 .
C1 Lu1 N2 N1 165.14(12) . .
C2 Lu1 N2 N1 -98.89(11) . .
N4 Lu1 N2 N1 62.67(11) . .
C11 N3 N4 C13 0.0 . .
B1 N3 N4 C13 180.0 . .
C11 N3 N4 Lu1 180.0 . .
B1 N3 N4 Lu1 0.0 . .
N2 Lu1 N4 C13 130.15(4) . .
N2 Lu1 N4 C13 -130.15(4) 7_575 .
C1 Lu1 N4 C13 0.0 . .
C2 Lu1 N4 C13 180.0 . .
N2 Lu1 N4 N3 -49.85(4) . .
N2 Lu1 N4 N3 49.85(4) 7_575 .
C1 Lu1 N4 N3 180.0 . .
C2 Lu1 N4 N3 0.0 . .
C11 N3 B1 N1 -117.80(14) . .
N4 N3 B1 N1 62.20(14) . .
C11 N3 B1 N1 117.80(14) . 7_575
N4 N3 B1 N1 -62.20(14) . 7_575
C3 N1 B1 N3 122.1(2) . .
N2 N1 B1 N3 -47.6(2) . .
C3 N1 B1 N1 -116.2(2) . 7_575
N2 N1 B1 N1 74.1(2) . 7_575
N2 N1 C3 C4 -0.6(2) . .
B1 N1 C3 C4 -171.34(19) . .
N2 N1 C3 C6 177.32(19) . .
B1 N1 C3 C6 6.5(3) . .
N1 C3 C4 C5 0.9(2) . .
C6 C3 C4 C5 -176.9(2) . .
N1 N2 C5 C4 0.5(2) . .
Lu1 N2 C5 C4 -155.84(15) . .
N1 N2 C5 C7 -175.01(16) . .
Lu1 N2 C5 C7 28.6(3) . .
C3 C4 C5 N2 -0.9(2) . .
C3 C4 C5 C7 174.32(19) . .
N2 C5 C7 C10 -5.5(3) . .
C4 C5 C7 C10 179.9(2) . .
N2 C5 C7 C8 -126.8(2) . .
C4 C5 C7 C8 58.5(3) . .
N2 C5 C7 C9 113.2(2) . .
C4 C5 C7 C9 -61.4(3) . .
N4 N3 C11 C12 0.0 . .
B1 N3 C11 C12 180.0 . .
N4 N3 C11 C14 180.0 . .
B1 N3 C11 C14 0.0 . .
N3 C11 C12 C13 0.0 . .
C14 C11 C12 C13 180.0 . .
N3 N4 C13 C12 0.0 . .
Lu1 N4 C13 C12 180.0 . .
N3 N4 C13 C15 180.0 . .
Lu1 N4 C13 C15 0.0 . .
C11 C12 C13 N4 0.0 . .
C11 C12 C13 C15 180.0 . .
N4 C13 C15 C16 60.52(17) . 7_575
C12 C13 C15 C16 -119.48(17) . 7_575
N4 C13 C15 C16 -60.52(17) . .
C12 C13 C15 C16 119.48(17) . .
N4 C13 C15 C18 180.0 . .
C12 C13 C15 C18 0.0 . .
