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#$Date: 2016-03-22 10:39:23 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178879 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/08/4110889.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_4110889
loop_
_publ_author_name
'Endre Szuromi'
'Jianguo Wu'
'Paul R. Sharp'
_publ_contact_author_address
;
 Department of Chemistry
 University of Missouri
 Columbia, MO  65211
;
_publ_contact_author_email       SharpP@missouri.edu
_publ_contact_author_fax         573-882-2754
_publ_contact_author_name        ' Paul R. Sharp'
_publ_contact_author_phone       573-882-7715
_publ_section_title
;
 Reversible Alkene Extrusion from Platinaoxetanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12088
_journal_page_last               12089
_journal_paper_doi               10.1021/ja065207s
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C11 H17 Cl O Pt'
_chemical_formula_sum            'C11 H17 Cl O Pt'
_chemical_formula_weight         395.79
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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            8
_cell_length_a                   8.2632(11)
_cell_length_b                   13.7649(17)
_cell_length_c                   19.649(3)
_cell_measurement_reflns_used    952
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.16
_cell_measurement_theta_min      3.05
_cell_volume                     2234.9(5)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics
;
 L. J. Barbour, X-Seed - Graphical Interface to
 SHELX-97 and POV-Ray, 1999
 ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997) 
;
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement
;
 SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to
 SHELX-97 and POV-Ray, 1999
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_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  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6475
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    12.760
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.353
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0278
_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)+(0.0263P)²+0.4555P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0596
_reflns_number_gt                1318
_reflns_number_total             1590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065207ssi20060720_112527_2.cif
_cod_data_source_block           CODPtCl(CH2COCH3)
_cod_database_code               4110889
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -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
Pt1 Pt 0.06904(3) 0.41779(2) 0.392678(14) 0.01660(13) Uani 1 1 d .
C4 C 0.3774(9) 0.2981(5) 0.4323(4) 0.0216(18) Uani 1 1 d .
H3A H 0.4551 0.2850 0.3951 0.026 Uiso 1 1 calc R
H3B H 0.4041 0.2540 0.4705 0.026 Uiso 1 1 calc R
Cl1 Cl -0.1819(2) 0.34601(14) 0.41085(10) 0.0276(5) Uani 1 1 d .
C8 C 0.3653(9) 0.4072(5) 0.2977(4) 0.0275(19) Uani 1 1 d .
H4A H 0.4704 0.3878 0.3177 0.033 Uiso 1 1 calc R
H4B H 0.3878 0.4411 0.2543 0.033 Uiso 1 1 calc R
C3 C 0.3983(9) 0.4029(5) 0.4560(4) 0.027(2) Uani 1 1 d .
H6A H 0.3672 0.4069 0.5046 0.033 Uiso 1 1 calc R
H6B H 0.5143 0.4202 0.4527 0.033 Uiso 1 1 calc R
C2 C 0.3016(8) 0.4770(6) 0.4168(4) 0.0233(18) Uani 1 1 d .
H7 H 0.2981 0.5428 0.4383 0.028 Uiso 1 1 calc R
C7 C 0.2644(9) 0.3140(5) 0.2825(4) 0.0249(19) Uani 1 1 d .
H8A H 0.1934 0.3267 0.2429 0.030 Uiso 1 1 calc R
H8B H 0.3392 0.2608 0.2700 0.030 Uiso 1 1 calc R
C1 C 0.2814(8) 0.4774(5) 0.3460(4) 0.0195(18) Uani 1 1 d .
H9 H 0.2649 0.5437 0.3264 0.023 Uiso 1 1 calc R
C6 C 0.1626(9) 0.2817(5) 0.3409(4) 0.0209(18) Uani 1 1 d .
H1 H 0.0754 0.2349 0.3278 0.025 Uiso 1 1 calc R
C5 C 0.2077(9) 0.2755(5) 0.4075(4) 0.0233(19) Uani 1 1 d .
H5 H 0.1490 0.2249 0.4345 0.028 Uiso 1 1 calc R
C9 C -0.0311(9) 0.5542(5) 0.4080(4) 0.0209(18) Uani 1 1 d .
H10A H -0.1099 0.5511 0.4459 0.025 Uiso 1 1 calc R
H10B H 0.0554 0.6005 0.4211 0.025 Uiso 1 1 calc R
O1 O -0.0375(6) 0.6299(4) 0.2988(3) 0.0340(15) Uani 1 1 d .
C11 C -0.2934(9) 0.5765(6) 0.3390(4) 0.029(2) Uani 1 1 d .
H2A H -0.3491 0.6250 0.3670 0.044 Uiso 1 1 calc R
H2B H -0.3225 0.5112 0.3546 0.044 Uiso 1 1 calc R
H2C H -0.3260 0.5844 0.2913 0.044 Uiso 1 1 calc R
C10 C -0.1146(9) 0.5903(5) 0.3450(4) 0.0240(19) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.01309(19) 0.01826(19) 0.0184(2) -0.00119(14) -0.00007(12) 0.00142(13)
C4 0.025(4) 0.021(4) 0.019(5) 0.009(4) 0.000(3) 0.008(3)
Cl1 0.0146(10) 0.0345(12) 0.0336(12) 0.0052(10) 0.0025(8) -0.0023(8)
C8 0.028(5) 0.027(5) 0.027(5) 0.006(4) 0.007(3) -0.003(4)
C3 0.018(4) 0.039(5) 0.025(5) -0.007(4) 0.000(3) -0.002(4)
C2 0.008(4) 0.027(5) 0.035(5) -0.001(4) -0.002(3) -0.005(3)
C7 0.025(5) 0.026(5) 0.024(5) -0.005(4) 0.004(3) 0.011(4)
C1 0.012(4) 0.015(4) 0.032(5) 0.001(4) 0.001(3) 0.003(3)
C6 0.018(4) 0.016(4) 0.028(5) -0.010(4) -0.002(3) 0.001(3)
C5 0.023(4) 0.020(5) 0.027(5) -0.001(4) 0.004(3) -0.003(3)
C9 0.021(4) 0.020(4) 0.021(5) -0.006(3) 0.000(3) 0.003(3)
O1 0.031(4) 0.036(3) 0.035(4) 0.013(3) 0.015(3) 0.003(3)
C11 0.019(4) 0.033(5) 0.036(5) 0.004(4) -0.007(3) 0.008(4)
C10 0.028(5) 0.015(4) 0.029(5) -0.011(4) 0.000(4) 0.008(4)
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'
Pt Pt -1.7033 8.3905 '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
C9 Pt1 C2 88.9(3)
C9 Pt1 C1 92.4(3)
C2 Pt1 C1 38.2(3)
C9 Pt1 C6 161.7(3)
C2 Pt1 C6 96.2(3)
C1 Pt1 C6 81.1(3)
C9 Pt1 C5 163.0(3)
C2 Pt1 C5 81.3(3)
C1 Pt1 C5 88.4(3)
C6 Pt1 C5 34.8(2)
C9 Pt1 Cl1 90.4(2)
C2 Pt1 Cl1 158.2(2)
C1 Pt1 Cl1 163.48(19)
C6 Pt1 Cl1 91.3(2)
C5 Pt1 Cl1 93.62(19)
C5 C4 C3 113.4(6)
C1 C8 C7 113.5(6)
C2 C3 C4 115.1(6)
C1 C2 C3 125.0(7)
C1 C2 Pt1 71.0(4)
C3 C2 Pt1 109.3(5)
C6 C7 C8 113.6(6)
C2 C1 C8 124.2(6)
C2 C1 Pt1 70.8(4)
C8 C1 Pt1 113.3(5)
C5 C6 C7 127.1(7)
C5 C6 Pt1 73.4(4)
C7 C6 Pt1 106.9(5)
C6 C5 C4 123.3(7)
C6 C5 Pt1 71.8(4)
C4 C5 Pt1 109.1(5)
C10 C9 Pt1 111.2(5)
O1 C10 C11 120.5(7)
O1 C10 C9 121.0(7)
C11 C10 C9 118.5(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pt1 C9 2.074(7)
Pt1 C2 2.140(7)
Pt1 C1 2.144(7)
Pt1 C6 2.267(7)
Pt1 C5 2.288(7)
Pt1 Cl1 2.3245(19)
C4 C5 1.518(10)
C4 C3 1.525(10)
C8 C1 1.521(10)
C8 C7 1.558(10)
C3 C2 1.507(10)
C2 C1 1.402(10)
C7 C6 1.490(10)
C6 C5 1.363(10)
C9 C10 1.503(11)
O1 C10 1.236(9)
C11 C10 1.495(10)
