#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:08:14 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178936 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/65/4116518.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_4116518
loop_
_publ_author_name
'Paul-Michael Pellny'
'Frank G. Kirchbauer'
'Vladimir V. Burlakov'
'Wolfgang Baumann'
'Anke Spannenberg'
'Uwe Rosenthal'
_publ_section_title
;
 Reactivity of Permethylzirconocene and Permethyltitanocene toward
 Disubstituted 1,3-Butadiynes: η4- vs η2-Complexation or C-C Coupling
 with the Permethyltitanocene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8313
_journal_page_last               8323
_journal_paper_doi               10.1021/ja991046z
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C32 H48 O4 Si2 Zr'
_chemical_formula_weight         644.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   17.104(3)
_cell_length_b                   17.173(3)
_cell_length_c                   48.170(10)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      4
_cell_volume                     14149(5)
_computing_cell_refinement       STOE-CELL
_computing_data_collection       STOE-EXPOSE
_computing_data_reduction        STOE-INTEGRATE
_computing_molecular_graphics    XP
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       STOE-IPDS
_diffrn_measurement_method       'LASER SCANNED IMAGING PLATE'
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10158
_diffrn_reflns_theta_max         24.33
_diffrn_reflns_theta_min         1.73
_diffrn_standards_interval_time  360
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_type   'MEAN IMAGING PLATE INTENSITY METHOD'
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             5440
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.976
_refine_ls_goodness_of_fit_obs   1.054
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_restrained_S_obs      1.054
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_obs          0.0345
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0643P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0925
_refine_ls_wR_factor_obs         0.0886
_reflns_number_observed          2275
_reflns_number_total             2848
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja991046z_6.cif
_cod_data_source_block           206
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        14148.8(46)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4116518
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.3112(2) 0.4999(2) 0.13214(5) 0.0395(6) Uani 1 d .
C2 C 0.3593(2) 0.5218(2) 0.10938(6) 0.0419(7) Uani 1 d .
C3 C 0.4380(2) 0.5104(2) 0.11741(6) 0.0440(7) Uani 1 d .
C4 C 0.4387(2) 0.4794(2) 0.14458(6) 0.0462(7) Uani 1 d .
C5 C 0.3602(2) 0.4741(2) 0.15383(5) 0.0426(7) Uani 1 d .
C6 C 0.3331(3) 0.4639(2) 0.18349(6) 0.0730(11) Uani 1 d .
H6A H 0.3759(3) 0.4460(2) 0.19468(6) 0.110 Uiso 1 calc R
H6B H 0.2915(3) 0.4265(2) 0.18409(6) 0.110 Uiso 1 calc R
H6C H 0.3147(3) 0.5129(2) 0.19053(6) 0.110 Uiso 1 calc R
C7 C 0.2616(2) 0.3882(2) 0.03906(5) 0.0410(6) Uani 1 d .
C8 C 0.2315(2) 0.3920(2) 0.06865(5) 0.0398(6) Uani 1 d .
C9 C 0.1117(3) 0.3251(3) 0.01223(9) 0.105(2) Uani 1 d .
H9A H 0.1350(3) 0.2744(3) 0.01092(9) 0.157 Uiso 1 calc R
H9B H 0.0750(3) 0.3319(3) -0.00266(9) 0.157 Uiso 1 calc R
H9C H 0.0850(3) 0.3300(3) 0.02968(9) 0.157 Uiso 1 calc R
C10 C 0.2438(2) 0.3875(2) -0.02333(6) 0.0748(11) Uani 1 d .
H10A H 0.2652(2) 0.3358(2) -0.02396(6) 0.112 Uiso 1 calc R
H10B H 0.2854(2) 0.4249(2) -0.02441(6) 0.112 Uiso 1 calc R
H10C H 0.2088(2) 0.3947(2) -0.03870(6) 0.112 Uiso 1 calc R
C11 C 0.1467(3) 0.4998(3) 0.01219(9) 0.0931(14) Uani 1 d .
H11A H 0.1191(3) 0.5050(3) 0.02945(9) 0.140 Uiso 1 calc R
H11B H 0.1111(3) 0.5078(3) -0.00295(9) 0.140 Uiso 1 calc R
H11C H 0.1877(3) 0.5380(3) 0.01134(9) 0.140 Uiso 1 calc R
C12 C 0.2235(2) 0.5076(2) 0.13351(7) 0.0633(9) Uani 1 d .
H12A H 0.2042(2) 0.5263(2) 0.11602(7) 0.095 Uiso 1 calc R
H12B H 0.2097(2) 0.5437(2) 0.14791(7) 0.095 Uiso 1 calc R
H12C H 0.2008(2) 0.4577(2) 0.13747(7) 0.095 Uiso 1 calc R
C13 C 0.5121(2) 0.4657(2) 0.16126(8) 0.0774(11) Uani 1 d .
H13A H 0.4986(2) 0.4444(2) 0.17904(8) 0.116 Uiso 1 calc R
H13B H 0.5391(2) 0.5142(2) 0.16380(8) 0.116 Uiso 1 calc R
H13C H 0.5454(2) 0.4299(2) 0.15155(8) 0.116 Uiso 1 calc R
C14 C 0.3381(2) 0.3789(2) 0.03579(5) 0.0440(6) Uani 1 d .
C15 C 0.3322(2) 0.5572(2) 0.08258(6) 0.0660(9) Uani 1 d .
H15A H 0.2761(2) 0.5583(2) 0.08221(6) 0.099 Uiso 1 calc R
H15B H 0.3511(2) 0.5266(2) 0.06730(6) 0.099 Uiso 1 calc R
H15C H 0.3520(2) 0.6093(2) 0.08108(6) 0.099 Uiso 1 calc R
C16 C 0.5088(2) 0.5325(2) 0.10049(8) 0.0751(11) Uani 1 d .
H16A H 0.4923(2) 0.5521(2) 0.08276(8) 0.113 Uiso 1 calc R
H16B H 0.5413(2) 0.4875(2) 0.09783(8) 0.113 Uiso 1 calc R
H16C H 0.5379(2) 0.5720(2) 0.11010(8) 0.113 Uiso 1 calc R
O1 O 0.28238(10) 0.38044(11) 0.08822(3) 0.0421(4) Uani 1 d .
O2 O 0.16212(12) 0.4046(2) 0.07260(4) 0.0640(6) Uani 1 d .
Si Si 0.18951(5) 0.40101(6) 0.00975(2) 0.0515(2) Uani 1 d .
Zr Zr 0.3750 0.3750 0.114755(6) 0.03004(14) Uani 1 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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
C5 C1 C2 108.0(2) . .
C5 C1 C12 125.9(3) . .
C2 C1 C12 125.9(3) . .
C5 C1 Zr 74.02(15) . .
C2 C1 Zr 73.80(15) . .
C12 C1 Zr 121.0(2) . .
C3 C2 C1 107.7(2) . .
C3 C2 C15 125.9(3) . .
C1 C2 C15 126.2(3) . .
C3 C2 Zr 74.6(2) . .
C1 C2 Zr 73.8(2) . .
C15 C2 Zr 121.4(2) . .
C4 C3 C2 108.3(2) . .
C4 C3 C16 126.1(3) . .
C2 C3 C16 125.5(3) . .
C4 C3 Zr 73.0(2) . .
C2 C3 Zr 73.3(2) . .
C16 C3 Zr 122.6(2) . .
C3 C4 C5 107.9(3) . .
C3 C4 C13 124.0(3) . .
C5 C4 C13 127.7(3) . .
C3 C4 Zr 74.9(2) . .
C5 C4 Zr 74.1(2) . .
C13 C4 Zr 123.2(2) . .
C1 C5 C4 108.1(2) . .
C1 C5 C6 123.6(3) . .
C4 C5 C6 126.5(3) . .
C1 C5 Zr 73.85(14) . .
C4 C5 Zr 73.53(15) . .
C6 C5 Zr 130.6(2) . .
C14 C7 C8 116.8(2) . .
C14 C7 Si 124.7(2) . .
C8 C7 Si 118.4(2) . .
O2 C8 O1 124.4(2) . .
O2 C8 C7 118.9(2) . .
O1 C8 C7 116.6(2) . .
C14 C14 C7 173.1(2) 2 .
C8 O1 Zr 169.6(2) . .
C11 Si C10 111.5(2) . .
C11 Si C9 110.7(2) . .
C10 Si C9 108.9(2) . .
C11 Si C7 108.5(2) . .
C10 Si C7 107.47(15) . .
C9 Si C7 109.7(2) . .
O1 Zr O1 102.30(10) . 2
O1 Zr C4 93.06(9) . 2
O1 Zr C4 130.95(9) 2 2
O1 Zr C4 130.95(8) . .
O1 Zr C4 93.06(9) 2 .
C4 Zr C4 111.19(14) 2 .
O1 Zr C1 80.47(8) . .
O1 Zr C1 125.30(8) 2 .
C4 Zr C1 102.93(9) 2 .
C4 Zr C1 53.46(9) . .
O1 Zr C1 125.31(8) . 2
O1 Zr C1 80.48(8) 2 2
C4 Zr C1 53.46(9) 2 2
C4 Zr C1 102.93(9) . 2
C1 Zr C1 141.61(12) . 2
O1 Zr C2 93.63(8) . 2
O1 Zr C2 79.00(8) 2 2
C4 Zr C2 53.50(9) 2 2
C4 Zr C2 135.21(9) . 2
C1 Zr C2 155.65(9) . 2
C1 Zr C2 32.41(9) 2 2
O1 Zr C2 79.00(8) . .
O1 Zr C2 93.63(8) 2 .
C4 Zr C2 135.21(9) 2 .
C4 Zr C2 53.50(9) . .
C1 Zr C2 32.41(9) . .
C1 Zr C2 155.65(9) 2 .
C2 Zr C2 168.34(12) 2 .
O1 Zr C5 110.81(8) . .
O1 Zr C5 124.79(8) 2 .
C4 Zr C5 90.63(9) 2 .
C4 Zr C5 32.33(9) . .
C1 Zr C5 32.14(9) . .
C1 Zr C5 111.19(9) 2 .
C2 Zr C5 138.21(9) 2 .
C2 Zr C5 53.44(9) . .
O1 Zr C5 124.80(8) . 2
O1 Zr C5 110.81(8) 2 2
C4 Zr C5 32.33(9) 2 2
C4 Zr C5 90.62(9) . 2
C1 Zr C5 111.19(9) . 2
C1 Zr C5 32.13(9) 2 2
C2 Zr C5 53.44(9) 2 2
C2 Zr C5 138.21(9) . 2
C5 Zr C5 84.86(12) . 2
O1 Zr C3 75.29(8) . 2
O1 Zr C3 108.44(9) 2 2
C4 Zr C3 32.12(9) 2 2
C4 Zr C3 142.25(9) . 2
C1 Zr C3 124.49(10) . 2
C1 Zr C3 53.21(9) 2 2
C2 Zr C3 32.10(9) 2 2
C2 Zr C3 149.01(9) . 2
C5 Zr C3 121.76(9) . 2
C5 Zr C3 53.15(9) 2 2
O1 Zr C3 108.44(9) . .
O1 Zr C3 75.29(8) 2 .
C4 Zr C3 142.25(9) 2 .
C4 Zr C3 32.11(9) . .
C1 Zr C3 53.21(9) . .
C1 Zr C3 124.48(10) 2 .
C2 Zr C3 149.01(9) 2 .
C2 Zr C3 32.10(9) . .
C5 Zr C3 53.14(9) . .
C5 Zr C3 121.75(9) 2 .
C3 Zr C3 174.29(12) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C5 1.411(4) .
C1 C2 1.422(4) .
C1 C12 1.506(4) .
C1 Zr 2.548(3) .
C2 C3 1.414(4) .
C2 C15 1.501(4) .
C2 Zr 2.548(3) .
C3 C4 1.413(4) .
C3 C16 1.508(4) .
C3 Zr 2.566(3) .
C4 C5 1.418(4) .
C4 C13 1.509(4) .
C4 Zr 2.542(3) .
C5 C6 1.513(4) .
C5 Zr 2.550(3) .
C7 C14 1.328(4) .
C7 C8 1.517(4) .
C7 Si 1.888(3) .
C8 O2 1.221(3) .
C8 O1 1.298(3) .
C9 Si 1.867(4) .
C10 Si 1.859(3) .
C11 Si 1.852(5) .
C14 C14 1.268(6) 2
O1 Zr 2.038(2) .
Zr O1 2.038(2) 2
Zr C4 2.542(3) 2
Zr C1 2.548(3) 2
Zr C2 2.548(3) 2
Zr C5 2.550(3) 2
Zr C3 2.566(3) 2
