#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/20/7052046.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_7052046
loop_
_publ_author_name
'Marc D. Walter'
'Dirk Bentz'
'Frank Weber'
'Oliver Schmitt'
'Gotthelf Wolmershäuser'
'Helmut Sitzmann'
_publ_section_title
;
 Cation size dependent reactivity of lanthanide trihalides with bulky
 alkylcyclopentadienyl anions
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              305
_journal_paper_doi               10.1039/b603701a
_journal_volume                  31
_journal_year                    2007
_chemical_formula_sum            'C21 H39 Cl2 O2 Tm'
_chemical_formula_weight         563.35
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 105.603(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8947(6)
_cell_length_b                   13.8338(7)
_cell_length_c                   10.3037(8)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2
_cell_volume                     1221.12(15)
_computing_cell_refinement       'Stoe IPDS V2.63'
_computing_data_collection       'Stoe IPDS V2.63'
_computing_data_reduction        'Stoe IPDS V2.63'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       Phi-Oscillation
_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  0.1315
_diffrn_reflns_av_sigmaI/netI    0.0951
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17167
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    3.863
_exptl_absorpt_correction_T_max  0.717
_exptl_absorpt_correction_T_min  0.364
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(ABST/PLATON 99)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4553
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0228P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0745
_reflns_number_gt                3573
_reflns_number_total             4553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b603701a.txt
_cod_data_source_block           0129
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1221.12(14)
_cod_original_sg_symbol_Hall     P_2yb
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7052046
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm Tm 0.07600(4) 0.2462 0.31509(3) 0.03329(9) Uani 1 d . . .
Cl1 Cl -0.0775(3) 0.10644(17) 0.1825(3) 0.0565(6) Uani 1 d . . .
Cl2 Cl 0.1061(3) 0.16000(18) 0.5363(3) 0.0542(6) Uani 1 d . . .
O1 O -0.1794(8) 0.3197(5) 0.2513(7) 0.0565(18) Uani 1 d . . .
O2 O 0.0534(9) 0.3863(5) 0.4509(7) 0.0573(19) Uani 1 d . . .
C1 C 0.3787(9) 0.2255(6) 0.3493(8) 0.028(3) Uani 1 d . . .
C2 C 0.3086(13) 0.1798(8) 0.2242(12) 0.037(3) Uani 1 d . . .
C3 C 0.2352(9) 0.2578(11) 0.1298(7) 0.031(2) Uani 1 d . . .
C4 C 0.2607(12) 0.3441(8) 0.1989(10) 0.033(2) Uani 1 d . . .
C5 C 0.3469(10) 0.3266(7) 0.3309(9) 0.033(2) Uani 1 d . . .
H5 H 0.3790 0.3736 0.3972 0.040 Uiso 1 calc R . .
C6 C -0.3037(13) 0.3048(9) 0.1391(12) 0.080(4) Uani 1 d . . .
H6A H -0.3999 0.3109 0.1638 0.120 Uiso 1 calc R . .
H6B H -0.2967 0.2411 0.1040 0.120 Uiso 1 calc R . .
H6C H -0.3007 0.3520 0.0715 0.120 Uiso 1 calc R . .
C7 C -0.2101(14) 0.3987(8) 0.3294(15) 0.077(4) Uani 1 d . . .
H7A H -0.1972 0.4594 0.2864 0.092 Uiso 1 calc R . .
H7B H -0.3167 0.3952 0.3361 0.092 Uiso 1 calc R . .
C8 C -0.0993(15) 0.3942(8) 0.4666(15) 0.076(4) Uani 1 d . . .
H8A H -0.1083 0.4521 0.5170 0.092 Uiso 1 calc R . .
H8B H -0.1228 0.3387 0.5153 0.092 Uiso 1 calc R . .
C9 C 0.1618(15) 0.4168(9) 0.5696(10) 0.077(4) Uani 1 d . . .
H9A H 0.1445 0.4838 0.5853 0.115 Uiso 1 calc R . .
H9B H 0.2657 0.4085 0.5605 0.115 Uiso 1 calc R . .
H9C H 0.1494 0.3790 0.6441 0.115 Uiso 1 calc R . .
C11 C 0.4844(11) 0.1841(6) 0.4761(9) 0.044(2) Uani 1 d . . .
H11 H 0.4351 0.1247 0.4966 0.053 Uiso 1 calc R . .
C12 C 0.5093(11) 0.2495(17) 0.5985(8) 0.071(3) Uani 1 d . . .
H12A H 0.5177 0.3154 0.5718 0.106 Uiso 1 calc R . .
H12B H 0.6035 0.2311 0.6643 0.106 Uiso 1 calc R . .
H12C H 0.4224 0.2434 0.6366 0.106 Uiso 1 calc R . .
C13 C 0.6445(12) 0.1554(8) 0.4564(14) 0.078(4) Uani 1 d . . .
H13A H 0.7135 0.2100 0.4751 0.117 Uiso 1 calc R . .
H13B H 0.6315 0.1347 0.3651 0.117 Uiso 1 calc R . .
H13C H 0.6881 0.1035 0.5167 0.117 Uiso 1 calc R . .
C21 C 0.3061(13) 0.0750(7) 0.1842(11) 0.046(2) Uani 1 d . . .
H21 H 0.2073 0.0647 0.1153 0.055 Uiso 1 calc R . .
C22 C 0.3111(13) 0.0002(7) 0.2962(12) 0.066(3) Uani 1 d . . .
H22A H 0.4134 -0.0002 0.3581 0.100 Uiso 1 calc R . .
H22B H 0.2878 -0.0628 0.2568 0.100 Uiso 1 calc R . .
H22C H 0.2354 0.0171 0.3434 0.100 Uiso 1 calc R . .
C23 C 0.4395(14) 0.0537(8) 0.1150(14) 0.079(4) Uani 1 d . . .
H23A H 0.4189 0.0878 0.0309 0.118 Uiso 1 calc R . .
H23B H 0.4438 -0.0144 0.0989 0.118 Uiso 1 calc R . .
H23C H 0.5376 0.0748 0.1729 0.118 Uiso 1 calc R . .
C31 C 0.1635(10) 0.2417(18) -0.0204(7) 0.056(2) Uani 1 d . . .
H31 H 0.1544 0.1713 -0.0308 0.067 Uiso 1 calc R . .
C32 C 0.0029(15) 0.2788(8) -0.0806(11) 0.084(5) Uani 1 d . . .
H32A H -0.0581 0.2711 -0.0174 0.126 Uiso 1 calc R . .
H32B H -0.0445 0.2432 -0.1613 0.126 Uiso 1 calc R . .
H32C H 0.0077 0.3460 -0.1022 0.126 Uiso 1 calc R . .
C33 C 0.2801(15) 0.2714(9) -0.0990(9) 0.080(5) Uani 1 d . . .
H33A H 0.2959 0.3400 -0.0922 0.119 Uiso 1 calc R . .
H33B H 0.2396 0.2537 -0.1920 0.119 Uiso 1 calc R . .
H33C H 0.3777 0.2389 -0.0621 0.119 Uiso 1 calc R . .
C41 C 0.2218(12) 0.4446(7) 0.1357(10) 0.045(2) Uani 1 d . . .
H41 H 0.1920 0.4363 0.0376 0.054 Uiso 1 calc R . .
C42 C 0.0853(15) 0.4938(8) 0.1731(15) 0.089(5) Uani 1 d . . .
H42A H 0.1100 0.5016 0.2691 0.133 Uiso 1 calc R . .
H42B H -0.0067 0.4547 0.1431 0.133 Uiso 1 calc R . .
H42C H 0.0670 0.5561 0.1306 0.133 Uiso 1 calc R . .
C43 C 0.3628(13) 0.5117(8) 0.1717(14) 0.075(4) Uani 1 d . . .
H43A H 0.4013 0.5161 0.2680 0.112 Uiso 1 calc R . .
H43B H 0.3327 0.5747 0.1350 0.112 Uiso 1 calc R . .
H43C H 0.4431 0.4864 0.1350 0.112 Uiso 1 calc R . .
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'
Tm Tm -0.3139 5.2483 '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 Tm O2 66.6(2) . . ?
O1 Tm Cl2 107.97(17) . . ?
O2 Tm Cl2 82.1(2) . . ?
O1 Tm Cl1 81.02(18) . . ?
O2 Tm Cl1 143.14(18) . . ?
Cl2 Tm Cl1 92.13(9) . . ?
O1 Tm C1 159.3(2) . . ?
O2 Tm C1 104.5(3) . . ?
Cl2 Tm C1 88.37(18) . . ?
Cl1 Tm C1 111.77(19) . . ?
O1 Tm C5 128.4(3) . . ?
O2 Tm C5 80.9(2) . . ?
Cl2 Tm C5 105.8(2) . . ?
Cl1 Tm C5 135.1(2) . . ?
C1 Tm C5 31.6(3) . . ?
O1 Tm C4 108.3(3) . . ?
O2 Tm C4 90.6(3) . . ?
Cl2 Tm C4 136.2(2) . . ?
Cl1 Tm C4 117.0(2) . . ?
C1 Tm C4 51.8(3) . . ?
C5 Tm C4 30.6(3) . . ?
O1 Tm C2 144.7(3) . . ?
O2 Tm C2 132.2(3) . . ?
Cl2 Tm C2 104.6(3) . . ?
Cl1 Tm C2 84.5(2) . . ?
C1 Tm C2 31.1(3) . . ?
C5 Tm C2 51.5(3) . . ?
C4 Tm C2 51.8(3) . . ?
O1 Tm C3 114.9(3) . . ?
O2 Tm C3 120.4(4) . . ?
Cl2 Tm C3 136.6(3) . . ?
Cl1 Tm C3 88.5(3) . . ?
C1 Tm C3 51.9(2) . . ?
C5 Tm C3 50.4(3) . . ?
C4 Tm C3 30.0(4) . . ?
C2 Tm C3 32.3(4) . . ?
C6 O1 C7 110.8(9) . . ?
C6 O1 Tm 130.3(6) . . ?
C7 O1 Tm 118.6(7) . . ?
C8 O2 C9 109.4(8) . . ?
C8 O2 Tm 111.0(6) . . ?
C9 O2 Tm 126.7(7) . . ?
C2 C1 C5 107.0(8) . . ?
C2 C1 C11 129.7(9) . . ?
C5 C1 C11 122.9(8) . . ?
C2 C1 Tm 75.1(5) . . ?
C5 C1 Tm 73.6(5) . . ?
C11 C1 Tm 122.4(5) . . ?
C3 C2 C1 106.2(9) . . ?
C3 C2 C21 123.4(10) . . ?
C1 C2 C21 130.4(11) . . ?
C3 C2 Tm 74.4(5) . . ?
C1 C2 Tm 73.7(5) . . ?
C21 C2 Tm 118.3(6) . . ?
C4 C3 C2 108.1(9) . . ?
C4 C3 C31 128.2(14) . . ?
C2 C3 C31 123.4(14) . . ?
C4 C3 Tm 74.2(5) . . ?
C2 C3 Tm 73.2(5) . . ?
C31 C3 Tm 124.0(5) . . ?
C3 C4 C5 109.0(10) . . ?
C3 C4 C41 125.4(9) . . ?
C5 C4 C41 125.1(10) . . ?
C3 C4 Tm 75.8(6) . . ?
C5 C4 Tm 73.4(5) . . ?
C41 C4 Tm 123.9(6) . . ?
C4 C5 C1 109.7(9) . . ?
C4 C5 Tm 76.0(6) . . ?
C1 C5 Tm 74.9(5) . . ?
C8 C7 O1 108.9(8) . . ?
O2 C8 C7 107.7(9) . . ?
C12 C11 C1 114.3(9) . . ?
C12 C11 C13 109.2(9) . . ?
C1 C11 C13 111.5(8) . . ?
C2 C21 C23 110.4(8) . . ?
C2 C21 C22 116.5(9) . . ?
C23 C21 C22 109.9(9) . . ?
C3 C31 C33 109.8(9) . . ?
C3 C31 C32 117.8(11) . . ?
C33 C31 C32 113.4(11) . . ?
C43 C41 C4 111.8(9) . . ?
C43 C41 C42 108.9(9) . . ?
C4 C41 C42 113.6(7) . . ?
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
Tm O1 2.414(6) . ?
Tm O2 2.430(6) . ?
Tm Cl2 2.522(2) . ?
Tm Cl1 2.542(2) . ?
Tm C1 2.636(8) . ?
Tm C5 2.619(9) . ?
Tm C4 2.651(10) . ?
Tm C2 2.654(10) . ?
Tm C3 2.670(6) . ?
O1 C6 1.383(13) . ?
O1 C7 1.427(12) . ?
O2 C8 1.415(12) . ?
O2 C9 1.403(13) . ?
C1 C2 1.420(14) . ?
C1 C5 1.430(14) . ?
C1 C11 1.503(12) . ?
C2 C3 1.482(17) . ?
C2 C21 1.505(13) . ?
C3 C4 1.377(18) . ?
C3 C31 1.524(11) . ?
C4 C5 1.391(13) . ?
C4 C41 1.535(13) . ?
C7 C8 1.491(18) . ?
C11 C12 1.519(17) . ?
C11 C13 1.544(12) . ?
C21 C23 1.568(12) . ?
C21 C22 1.541(14) . ?
C31 C33 1.534(12) . ?
C31 C32 1.487(16) . ?
C41 C43 1.523(14) . ?
C41 C42 1.529(13) . ?
