#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:12:22 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178619 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/30/4073030.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_4073030
loop_
_publ_author_name
'Jaroschik, Florian'
'Nief, François'
'Le Goff, Xavier-Frédéric'
'Ricard, Louis'
_publ_section_title
;
 Isolation of Stable Organodysprosium(II) Complexes by Chemical Reduction
 of Dysprosium(III) Precursors
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1123
_journal_paper_doi               10.1021/om0700213
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C34 H62 B Dy'
_chemical_formula_weight         644.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 102.5920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4490(10)
_cell_length_b                   16.3910(10)
_cell_length_c                   19.9810(10)
_cell_measurement_reflns_used    3234
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     3339.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  KappaCCD
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7866
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    2.256
_exptl_absorpt_correction_T_max  0.7430
_exptl_absorpt_correction_T_min  0.6367
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.987
_refine_diff_density_min         -1.479
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.0021(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0332
_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)+(0.0537P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                4333
_reflns_number_total             4840
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0700213si20070109_034632.cif
_cod_data_source_block           dyttcpbh4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C2/c     '
_cod_database_code               4073030
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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
Dy1 Dy 0.0000 0.143408(8) 0.2500 0.02597(8) Uani 1 2 d S
C1 C -0.1939(3) 0.14265(14) 0.13138(15) 0.0299(6) Uani 1 1 d .
C2 C -0.1733(2) 0.22688(16) 0.15225(12) 0.0286(5) Uani 1 1 d .
C3 C -0.0421(2) 0.24703(16) 0.14712(12) 0.0302(5) Uani 1 1 d .
H3 H -0.0018 0.2987 0.1582 0.036 Uiso 1 1 calc R
C4 C 0.0183(2) 0.17978(18) 0.12348(13) 0.0323(5) Uani 1 1 d .
C5 C -0.0731(3) 0.1158(2) 0.11639(14) 0.0346(6) Uani 1 1 d .
H5 H -0.0567 0.0617 0.1033 0.042 Uiso 1 1 calc R
C6 C -0.3171(3) 0.08830(18) 0.11225(15) 0.0383(6) Uani 1 1 d .
C7 C -0.2829(3) 0.0065(2) 0.0822(2) 0.0593(10) Uani 1 1 d .
H7A H -0.2170 -0.0223 0.1165 0.089 Uiso 1 1 calc R
H7B H -0.2480 0.0168 0.0413 0.089 Uiso 1 1 calc R
H7C H -0.3621 -0.0271 0.0698 0.089 Uiso 1 1 calc R
C8 C -0.3801(3) 0.06552(17) 0.17243(17) 0.0400(6) Uani 1 1 d .
H8A H -0.4550 0.0292 0.1561 0.060 Uiso 1 1 calc R
H8B H -0.4103 0.1151 0.1916 0.060 Uiso 1 1 calc R
H8C H -0.3154 0.0377 0.2079 0.060 Uiso 1 1 calc R
C9 C -0.4204(4) 0.1295(2) 0.05505(19) 0.0510(9) Uani 1 1 d .
H9A H -0.3789 0.1468 0.0179 0.077 Uiso 1 1 calc R
H9B H -0.4569 0.1773 0.0738 0.077 Uiso 1 1 calc R
H9C H -0.4909 0.0907 0.0372 0.077 Uiso 1 1 calc R
C10 C -0.2668(2) 0.29699(16) 0.16037(14) 0.0339(5) Uani 1 1 d .
C11 C -0.3875(3) 0.27342(17) 0.18853(17) 0.0418(7) Uani 1 1 d .
H11A H -0.4429 0.2360 0.1565 0.063 Uiso 1 1 calc R
H11B H -0.4376 0.3226 0.1939 0.063 Uiso 1 1 calc R
H11C H -0.3588 0.2467 0.2332 0.063 Uiso 1 1 calc R
C12 C -0.3122(4) 0.3382(2) 0.0900(2) 0.0558(9) Uani 1 1 d .
H12A H -0.3571 0.2981 0.0566 0.084 Uiso 1 1 calc R
H12B H -0.2359 0.3599 0.0748 0.084 Uiso 1 1 calc R
H12C H -0.3726 0.3829 0.0938 0.084 Uiso 1 1 calc R
C13 C -0.1935(4) 0.36328(15) 0.2094(2) 0.0427(8) Uani 1 1 d .
H13A H -0.2563 0.4041 0.2182 0.064 Uiso 1 1 calc R
H13B H -0.1279 0.3897 0.1883 0.064 Uiso 1 1 calc R
H13C H -0.1497 0.3379 0.2528 0.064 Uiso 1 1 calc R
C14 C 0.1523(3) 0.1754(2) 0.10594(14) 0.0366(6) Uani 1 1 d .
C15 C 0.1416(5) 0.1343(3) 0.0364(2) 0.0643(13) Uani 1 1 d .
H15A H 0.2286 0.1315 0.0257 0.096 Uiso 1 1 calc R
H15B H 0.0827 0.1660 0.0010 0.096 Uiso 1 1 calc R
H15C H 0.1066 0.0790 0.0380 0.096 Uiso 1 1 calc R
C16 C 0.2100(3) 0.2601(2) 0.10252(19) 0.0516(8) Uani 1 1 d .
H16A H 0.2955 0.2555 0.0902 0.077 Uiso 1 1 calc R
H16B H 0.2209 0.2867 0.1473 0.077 Uiso 1 1 calc R
H16C H 0.1509 0.2926 0.0678 0.077 Uiso 1 1 calc R
C17 C 0.2438(3) 0.1257(3) 0.1607(2) 0.0543(9) Uani 1 1 d .
H17A H 0.2146 0.0688 0.1583 0.081 Uiso 1 1 calc R
H17B H 0.2427 0.1480 0.2061 0.081 Uiso 1 1 calc R
H17C H 0.3332 0.1284 0.1530 0.081 Uiso 1 1 calc R
B1 B 0.0000 -0.0188(3) 0.2500 0.0405(10) Uani 1 2 d S
H1 H 0.082(3) 0.0261(19) 0.2428(15) 0.049 Uiso 1 1 d .
H2 H 0.033(3) -0.046(2) 0.2917(16) 0.049 Uiso 1 1 d .
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'
Dy Dy -0.1892 4.4098 '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
C3 Dy1 C3 99.50(12) 2 .
C3 Dy1 C4 30.84(8) 2 2
C3 Dy1 C4 124.56(9) . 2
C3 Dy1 C4 124.56(9) 2 .
C3 Dy1 C4 30.84(8) . .
C4 Dy1 C4 153.94(13) 2 .
C3 Dy1 C5 149.35(9) 2 .
C3 Dy1 C5 50.24(9) . .
C4 Dy1 C5 159.43(8) 2 .
C4 Dy1 C5 30.77(9) . .
C3 Dy1 C5 50.24(9) 2 2
C3 Dy1 C5 149.35(9) . 2
C4 Dy1 C5 30.77(9) 2 2
C4 Dy1 C5 159.43(8) . 2
C5 Dy1 C5 160.33(14) . 2
C3 Dy1 B1 130.25(6) 2 .
C3 Dy1 B1 130.25(6) . .
C4 Dy1 B1 103.03(6) 2 .
C4 Dy1 B1 103.03(6) . .
C5 Dy1 B1 80.17(7) . .
C5 Dy1 B1 80.17(7) 2 .
C3 Dy1 C2 31.04(7) 2 2
C3 Dy1 C2 102.00(8) . 2
C4 Dy1 C2 51.45(7) 2 2
C4 Dy1 C2 113.38(8) . 2
C5 Dy1 C2 143.92(8) . 2
C5 Dy1 C2 50.45(8) 2 2
B1 Dy1 C2 120.14(5) . 2
C3 Dy1 C2 102.00(8) 2 .
C3 Dy1 C2 31.04(7) . .
C4 Dy1 C2 113.38(8) 2 .
C4 Dy1 C2 51.45(7) . .
C5 Dy1 C2 50.45(8) . .
C5 Dy1 C2 143.92(8) 2 .
B1 Dy1 C2 120.14(5) . .
C2 Dy1 C2 119.72(11) 2 .
C3 Dy1 C1 50.62(8) 2 2
C3 Dy1 C1 129.82(8) . 2
C4 Dy1 C1 51.18(8) 2 2
C4 Dy1 C1 128.97(8) . 2
C5 Dy1 C1 149.30(8) . 2
C5 Dy1 C1 30.53(8) 2 2
B1 Dy1 C1 89.74(5) . 2
C2 Dy1 C1 30.52(7) 2 2
C2 Dy1 C1 149.99(8) . 2
C3 Dy1 C1 129.82(8) 2 .
C3 Dy1 C1 50.62(8) . .
C4 Dy1 C1 128.97(8) 2 .
C4 Dy1 C1 51.18(8) . .
C5 Dy1 C1 30.53(8) . .
C5 Dy1 C1 149.30(8) 2 .
B1 Dy1 C1 89.74(5) . .
C2 Dy1 C1 149.99(8) 2 .
C2 Dy1 C1 30.52(7) . .
C1 Dy1 C1 179.48(10) 2 .
C3 Dy1 H1 129.6(8) 2 .
C3 Dy1 H1 122.3(8) . .
C4 Dy1 H1 112.5(8) 2 .
C4 Dy1 H1 91.5(8) . .
C5 Dy1 H1 79.0(8) . .
C5 Dy1 H1 83.2(8) 2 .
B1 Dy1 H1 25.0(9) . .
C2 Dy1 H1 106.8(8) 2 .
C2 Dy1 H1 128.4(8) . .
C1 Dy1 H1 79.8(8) 2 .
C1 Dy1 H1 99.7(8) . .
C5 C1 C2 105.8(2) . .
C5 C1 C6 119.8(2) . .
C2 C1 C6 133.4(2) . .
C5 C1 Dy1 70.42(15) . .
C2 C1 Dy1 73.30(14) . .
C6 C1 Dy1 129.14(19) . .
C3 C2 C1 106.5(2) . .
C3 C2 C10 118.3(2) . .
C1 C2 C10 133.3(2) . .
C3 C2 Dy1 70.78(13) . .
C1 C2 Dy1 76.17(15) . .
C10 C2 Dy1 129.58(16) . .
C4 C3 C2 110.5(2) . .
C4 C3 Dy1 75.20(15) . .
C2 C3 Dy1 78.17(14) . .
C4 C3 H3 124.8 . .
C2 C3 H3 124.8 . .
Dy1 C3 H3 113.8 . .
C3 C4 C5 106.0(2) . .
C3 C4 C14 128.4(3) . .
C5 C4 C14 125.6(3) . .
C3 C4 Dy1 73.96(14) . .
C5 C4 Dy1 74.87(15) . .
C14 C4 Dy1 118.22(17) . .
C4 C5 C1 111.2(3) . .
C4 C5 Dy1 74.37(15) . .
C1 C5 Dy1 79.05(16) . .
C4 C5 H5 124.4 . .
C1 C5 H5 124.4 . .
Dy1 C5 H5 114.0 . .
C8 C6 C7 105.5(3) . .
C8 C6 C1 115.0(2) . .
C7 C6 C1 110.3(2) . .
C8 C6 C9 109.6(2) . .
C7 C6 C9 106.0(3) . .
C1 C6 C9 109.9(3) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C6 C9 H9A 109.5 . .
C6 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C6 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C11 C10 C12 109.3(3) . .
C11 C10 C2 116.2(2) . .
C12 C10 C2 107.9(2) . .
C11 C10 C13 106.1(2) . .
C12 C10 C13 106.3(3) . .
C2 C10 C13 110.6(2) . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C10 C13 H13A 109.5 . .
C10 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C10 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C4 C14 C16 111.2(3) . .
C4 C14 C17 109.0(2) . .
C16 C14 C17 109.1(3) . .
C4 C14 C15 110.1(3) . .
C16 C14 C15 108.2(3) . .
C17 C14 C15 109.2(3) . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C14 C16 H16A 109.5 . .
C14 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C14 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C14 C17 H17A 109.5 . .
C14 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C14 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
Dy1 B1 H1 50.6(16) . .
Dy1 B1 H2 118(2) . .
H1 B1 H2 106(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 C3 2.629(2) 2
Dy1 C3 2.629(2) .
Dy1 C4 2.644(2) 2
Dy1 C4 2.644(2) .
Dy1 C5 2.651(3) .
Dy1 C5 2.651(3) 2
Dy1 B1 2.660(4) .
Dy1 C2 2.725(2) 2
Dy1 C2 2.725(2) .
Dy1 C1 2.762(3) 2
Dy1 C1 2.762(3) .
Dy1 H1 2.12(3) .
C1 C5 1.429(4) .
C1 C2 1.445(3) .
C1 C6 1.543(4) .
C2 C3 1.436(3) .
C2 C10 1.540(3) .
C3 C4 1.402(4) .
C3 H3 0.9500 .
C4 C5 1.405(4) .
C4 C14 1.517(3) .
C5 H5 0.9500 .
C6 C8 1.538(4) .
C6 C7 1.543(4) .
C6 C9 1.546(4) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
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 C11 1.537(4) .
C10 C12 1.539(5) .
C10 C13 1.550(4) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 C16 1.521(5) .
C14 C17 1.523(4) .
C14 C15 1.525(5) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
B1 H1 1.16(3) .
B1 H2 0.94(3) .
