#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:59:01 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178631 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/42/4074273.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_4074273
loop_
_publ_author_name
'Vicente, José'
'Arcas, Aurelia'
'Fernández-Hernández, Jesús M.'
'Bautista, Delia'
_publ_section_title
;
 The First Family of Platinum(IV) Acetonyl Complexes. Mono-, Bis-, and
 Tris(acetonyl) Derivatives†
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4404
_journal_paper_doi               10.1021/om0605027
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C19 H23 Cl N2 O3 Pt'
_chemical_formula_weight         557.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     PATTERSON
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.032(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7305(5)
_cell_length_b                   27.1799(19)
_cell_length_c                   9.7153(7)
_cell_measurement_reflns_used    7287
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      2.37
_cell_volume                     1905.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       ω-scan
_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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20958
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    7.526
_exptl_absorpt_correction_T_max  0.5843
_exptl_absorpt_correction_T_min  0.1672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.945
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.391
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         4167
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0224
_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)+(0.0164P)²+4.1234P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0509
_reflns_number_gt                3991
_reflns_number_total             4167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0605027si20060606_015614.cif
_cod_data_source_block           533jmfins
_cod_original_sg_symbol_H-M      'P 2(1)/n'
_cod_database_code               4074273
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Pt1 Pt 0.082348(16) 0.112027(4) 0.963822(12) 0.01355(5) Uani 1 1 d .
Cl1 Cl 0.18341(11) 0.14511(3) 0.77232(9) 0.01949(16) Uani 1 1 d .
N1 N 0.2904(4) 0.15947(10) 1.1057(3) 0.0153(5) Uani 1 1 d D
N2 N -0.0715(4) 0.17633(10) 0.9675(3) 0.0159(5) Uani 1 1 d D
O1 O 0.5395(3) 0.06399(10) 0.9739(3) 0.0248(5) Uani 1 1 d .
O2 O -0.3077(4) 0.13298(10) 0.6351(3) 0.0292(6) Uani 1 1 d .
O3 O 0.0259(3) 0.14723(10) 1.3015(3) 0.0250(6) Uani 1 1 d .
C1 C 0.2342(5) 0.20698(12) 1.1035(3) 0.0163(6) Uani 1 1 d D
C2 C 0.3617(5) 0.24416(13) 1.1640(4) 0.0186(7) Uani 1 1 d D
H2 H 0.3220 0.2774 1.1580 0.022 Uiso 1 1 calc R
C3 C 0.5465(5) 0.23253(13) 1.2332(4) 0.0202(7) Uani 1 1 d D
H3 H 0.6348 0.2577 1.2762 0.024 Uiso 1 1 calc R
C4 C 0.6023(5) 0.18404(14) 1.2394(4) 0.0215(7) Uani 1 1 d D
H4 H 0.7283 0.1752 1.2890 0.026 Uiso 1 1 calc R
C5 C 0.4704(5) 0.14865(13) 1.1717(4) 0.0187(7) Uani 1 1 d D
H5 H 0.5090 0.1155 1.1720 0.022 Uiso 1 1 calc R
C6 C 0.0314(5) 0.21546(12) 1.0360(3) 0.0169(6) Uani 1 1 d D
C7 C -0.0503(5) 0.25990(13) 1.0487(3) 0.0197(7) Uani 1 1 d D
H7 H 0.0245 0.2872 1.0952 0.024 Uiso 1 1 calc R
C8 C -0.2410(5) 0.26404(14) 0.9930(4) 0.0230(7) Uani 1 1 d D
H8 H -0.2992 0.2944 0.9986 0.028 Uiso 1 1 calc R
C9 C -0.3459(5) 0.22328(14) 0.9290(4) 0.0218(7) Uani 1 1 d D
H9 H -0.4773 0.2250 0.8928 0.026 Uiso 1 1 calc R
C10 C -0.2579(5) 0.17992(13) 0.9180(3) 0.0191(7) Uani 1 1 d D
H10 H -0.3307 0.1520 0.8744 0.023 Uiso 1 1 calc R
C11 C 0.2471(4) 0.04958(12) 0.9957(4) 0.0164(6) Uani 1 1 d .
H11A H 0.3178 0.0460 1.1026 0.020 Uiso 1 1 calc R
H11B H 0.1650 0.0205 0.9639 0.020 Uiso 1 1 calc R
C12 C 0.3814(5) 0.04890(13) 0.9164(4) 0.0196(7) Uani 1 1 d .
C13 C 0.3179(5) 0.02559(15) 0.7661(4) 0.0270(8) Uani 1 1 d .
H13A H 0.4015 0.0352 0.7152 0.032 Uiso 1 1 calc R
H13B H 0.1918 0.0366 0.7089 0.032 Uiso 1 1 calc R
H13C H 0.3192 -0.0103 0.7763 0.032 Uiso 1 1 calc R
C14 C -0.1343(4) 0.07272(12) 0.8108(4) 0.0169(7) Uani 1 1 d .
H14A H -0.0898 0.0393 0.8004 0.020 Uiso 1 1 calc R
H14B H -0.2362 0.0693 0.8492 0.020 Uiso 1 1 calc R
C15 C -0.2096(5) 0.09670(14) 0.6600(4) 0.0206(7) Uani 1 1 d .
C16 C -0.1670(6) 0.07307(16) 0.5348(4) 0.0297(9) Uani 1 1 d .
H16A H -0.2506 0.0863 0.4406 0.036 Uiso 1 1 calc R
H16B H -0.1844 0.0374 0.5368 0.036 Uiso 1 1 calc R
H16C H -0.0384 0.0802 0.5459 0.036 Uiso 1 1 calc R
C17 C -0.0078(5) 0.08352(13) 1.1269(3) 0.0176(7) Uani 1 1 d .
H17A H -0.1436 0.0878 1.0964 0.021 Uiso 1 1 calc R
H17B H 0.0197 0.0479 1.1388 0.021 Uiso 1 1 calc R
C18 C 0.0868(5) 0.10919(13) 1.2702(4) 0.0194(7) Uani 1 1 d .
C19 C 0.2584(5) 0.08591(16) 1.3799(4) 0.0300(9) Uani 1 1 d .
H19A H 0.3307 0.1110 1.4493 0.036 Uiso 1 1 calc R
H19B H 0.3337 0.0717 1.3274 0.036 Uiso 1 1 calc R
H19C H 0.2223 0.0599 1.4341 0.036 Uiso 1 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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C11 Pt1 C14 88.87(13)
C11 Pt1 C17 86.43(13)
C14 Pt1 C17 87.11(13)
C11 Pt1 N2 171.10(11)
C14 Pt1 N2 97.02(12)
C17 Pt1 N2 87.20(12)
C11 Pt1 N1 96.77(12)
C14 Pt1 N1 173.48(12)
C17 Pt1 N1 96.49(11)
N2 Pt1 N1 77.79(10)
C11 Pt1 Cl1 93.89(9)
C14 Pt1 Cl1 92.31(9)
C17 Pt1 Cl1 179.33(9)
N2 Pt1 Cl1 92.55(8)
N1 Pt1 Cl1 84.06(7)
C5 N1 C1 119.1(3)
C5 N1 Pt1 126.1(2)
C1 N1 Pt1 113.6(2)
C10 N2 C6 118.9(3)
C10 N2 Pt1 125.9(2)
C6 N2 Pt1 115.0(2)
N1 C1 C2 120.7(3)
N1 C1 C6 115.8(3)
C2 C1 C6 123.5(3)
C3 C2 C1 119.6(3)
C2 C3 C4 119.5(3)
C3 C4 C5 118.5(3)
N1 C5 C4 122.4(3)
N2 C6 C7 121.5(3)
N2 C6 C1 115.9(3)
C7 C6 C1 122.5(3)
C8 C7 C6 119.5(3)
C7 C8 C9 118.8(3)
C8 C9 C10 119.5(3)
N2 C10 C9 121.7(3)
C12 C11 Pt1 115.7(2)
O1 C12 C11 121.8(3)
O1 C12 C13 120.7(3)
C11 C12 C13 117.4(3)
C15 C14 Pt1 113.5(2)
O2 C15 C16 119.1(3)
O2 C15 C14 122.5(3)
C16 C15 C14 118.4(3)
C18 C17 Pt1 110.4(2)
O3 C18 C17 121.7(3)
O3 C18 C19 120.0(3)
C17 C18 C19 118.3(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pt1 C11 2.078(3)
Pt1 C14 2.090(3)
Pt1 C17 2.095(3)
Pt1 N2 2.122(3)
Pt1 N1 2.135(3)
Pt1 Cl1 2.4338(8)
N1 C5 1.339(4)
N1 C1 1.360(4)
N2 C10 1.349(4)
N2 C6 1.352(4)
O1 C12 1.218(4)
O2 C15 1.214(5)
O3 C18 1.219(4)
C1 C2 1.386(5)
C1 C6 1.485(5)
C2 C3 1.380(5)
C3 C4 1.381(5)
C4 C5 1.384(5)
C6 C7 1.388(5)
C7 C8 1.381(5)
C8 C9 1.382(5)
C9 C10 1.384(5)
C11 C12 1.498(5)
C12 C13 1.503(5)
C14 C15 1.516(5)
C15 C16 1.512(5)
C17 C18 1.494(5)
C18 C19 1.510(5)
