#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:07:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179094 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/56/4305668.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_4305668
loop_
_publ_author_name
'José M. Casas'
'Beatriz E. Diosdado'
'Juan Forniés'
'Antonio Martín'
'Angel J. Rueda'
'A. Guy Orpen'
_publ_section_title
;
Synthesis of Binuclear Platinum Complexes Containing the Ligands
8-Naphthyridine, 2-Aminopyridine, and 7-Azaindolate. An Experimental Study
of the Steric Hindrance of the Bulky Pentafluorophenyl Ligands in the
Synthesis of Binuclear Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8767
_journal_page_last               8775
_journal_paper_doi               10.1021/ic8006475
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C20 H7 Cl F10 N2 O Pt'
_chemical_formula_weight         711.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.16(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.035(4)
_cell_length_b                   13.677(4)
_cell_length_c                   12.292(4)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      14.7
_cell_volume                     2082.3(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       'profile data from w 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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3853
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.973
_exptl_absorpt_correction_T_max  0.439
_exptl_absorpt_correction_T_min  0.360
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.625
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         3667
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0290
_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)+(0.0437P)²+0.9556P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                3072
_reflns_number_total             3667
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8006475_si_001_2.cif
_cod_data_source_block           4
_cod_original_cell_volume        2082.3(11)
_cod_database_code               4305668
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt Pt 0.342286(16) 0.188595(15) 0.205101(17) 0.02962(9) Uani 1 1 d . . .
Cl Cl 0.42777(13) 0.33636(11) 0.28793(14) 0.0463(4) Uani 1 1 d . . .
C1 C 0.2000(4) 0.2330(4) 0.2155(5) 0.0337(12) Uani 1 1 d . . .
C2 C 0.1472(5) 0.3130(4) 0.1563(5) 0.0390(13) Uani 1 1 d . . .
C3 C 0.0493(5) 0.3463(5) 0.1609(6) 0.0469(16) Uani 1 1 d . . .
C4 C -0.0009(5) 0.2973(5) 0.2263(6) 0.0502(17) Uani 1 1 d . . .
C5 C 0.0461(5) 0.2156(5) 0.2847(6) 0.0466(16) Uani 1 1 d . . .
C6 C 0.1446(5) 0.1856(5) 0.2797(5) 0.0406(14) Uani 1 1 d . . .
F2 F 0.1908(3) 0.3630(3) 0.0857(4) 0.0575(10) Uani 1 1 d . . .
F3 F 0.0031(3) 0.4261(3) 0.1016(4) 0.0755(13) Uani 1 1 d . . .
F4 F -0.0968(3) 0.3282(4) 0.2314(4) 0.0832(15) Uani 1 1 d . . .
F5 F -0.0043(4) 0.1660(4) 0.3480(4) 0.0771(14) Uani 1 1 d . . .
F6 F 0.1886(3) 0.1047(3) 0.3410(3) 0.0565(10) Uani 1 1 d . . .
C7 C 0.2724(4) 0.0637(4) 0.1362(5) 0.0343(12) Uani 1 1 d . . .
C8 C 0.1892(5) 0.0565(5) 0.0369(5) 0.0445(15) Uani 1 1 d . . .
C9 C 0.1400(6) -0.0306(6) -0.0057(6) 0.0552(19) Uani 1 1 d . . .
C10 C 0.1752(6) -0.1156(5) 0.0526(7) 0.0562(19) Uani 1 1 d . . .
C11 C 0.2584(6) -0.1122(5) 0.1512(6) 0.0496(17) Uani 1 1 d . . .
C12 C 0.3046(5) -0.0244(5) 0.1908(5) 0.0367(13) Uani 1 1 d . . .
F8 F 0.1489(4) 0.1367(3) -0.0253(4) 0.0694(12) Uani 1 1 d . . .
F9 F 0.0576(4) -0.0327(4) -0.1056(4) 0.0887(16) Uani 1 1 d . . .
F10 F 0.1295(4) -0.2019(4) 0.0113(5) 0.0906(16) Uani 1 1 d . . .
F11 F 0.2940(4) -0.1956(3) 0.2101(5) 0.0738(13) Uani 1 1 d . . .
F12 F 0.3865(3) -0.0268(3) 0.2917(3) 0.0515(9) Uani 1 1 d . . .
N1 N 0.4908(4) 0.1395(3) 0.1927(4) 0.0341(11) Uani 1 1 d . . .
N2 N 0.5609(4) 0.1278(4) 0.3903(4) 0.0393(12) Uani 1 1 d . . .
C13 C 0.5075(5) 0.1298(5) 0.0933(6) 0.0442(15) Uani 1 1 d . . .
C14 C 0.6055(6) 0.0985(6) 0.0793(6) 0.0580(19) Uani 1 1 d . . .
C15 C 0.6898(6) 0.0799(6) 0.1741(7) 0.0576(19) Uani 1 1 d . . .
C16 C 0.6777(5) 0.0905(5) 0.2819(6) 0.0424(15) Uani 1 1 d . . .
C17 C 0.7596(5) 0.0745(5) 0.3873(7) 0.0548(18) Uani 1 1 d . . .
C18 C 0.7386(6) 0.0844(6) 0.4872(7) 0.059(2) Uani 1 1 d . . .
C19 C 0.6379(6) 0.1105(6) 0.4875(6) 0.0532(18) Uani 1 1 d . . .
C20 C 0.5760(4) 0.1191(4) 0.2873(5) 0.0334(12) Uani 1 1 d . . .
O O 0.4115(4) 0.1360(5) 0.5143(4) 0.0719(15) Uani 1 1 d . . .
H2 H 0.507(6) 0.145(5) 0.398(6) 0.053(7) Uiso 1 1 d . . .
H13 H 0.446(5) 0.141(5) 0.033(6) 0.053(7) Uiso 1 1 d . . .
H14 H 0.614(5) 0.106(5) -0.010(5) 0.053(7) Uiso 1 1 d . . .
H15 H 0.760(5) 0.072(5) 0.176(6) 0.053(7) Uiso 1 1 d . . .
H17 H 0.830(5) 0.065(5) 0.382(5) 0.053(7) Uiso 1 1 d . . .
H18 H 0.794(5) 0.061(5) 0.550(6) 0.053(7) Uiso 1 1 d . . .
H19 H 0.618(5) 0.117(5) 0.547(6) 0.053(7) 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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
C1 Pt C7 88.7(2) . . ?
C1 Pt N1 179.0(2) . . ?
C7 Pt N1 90.3(2) . . ?
C1 Pt Cl 91.98(17) . . ?
C7 Pt Cl 179.28(17) . . ?
N1 Pt Cl 89.03(14) . . ?
C2 C1 C6 114.2(5) . . ?
C2 C1 Pt 122.1(4) . . ?
C6 C1 Pt 123.6(4) . . ?
F2 C2 C3 115.9(5) . . ?
F2 C2 C1 119.9(5) . . ?
C3 C2 C1 124.2(6) . . ?
F3 C3 C4 120.2(6) . . ?
F3 C3 C2 120.8(6) . . ?
C4 C3 C2 119.0(6) . . ?
F4 C4 C3 120.0(6) . . ?
F4 C4 C5 120.4(6) . . ?
C3 C4 C5 119.6(6) . . ?
F5 C5 C6 120.6(6) . . ?
F5 C5 C4 119.7(6) . . ?
C6 C5 C4 119.7(6) . . ?
F6 C6 C5 117.3(6) . . ?
F6 C6 C1 119.4(5) . . ?
C5 C6 C1 123.3(6) . . ?
C8 C7 C12 114.2(6) . . ?
C8 C7 Pt 125.0(5) . . ?
C12 C7 Pt 120.8(4) . . ?
F8 C8 C7 120.7(6) . . ?
F8 C8 C9 115.8(6) . . ?
C7 C8 C9 123.5(6) . . ?
F9 C9 C10 119.8(6) . . ?
F9 C9 C8 120.5(7) . . ?
C10 C9 C8 119.7(6) . . ?
F10 C10 C11 120.3(7) . . ?
F10 C10 C9 120.7(7) . . ?
C11 C10 C9 119.0(6) . . ?
F11 C11 C10 119.7(6) . . ?
F11 C11 C12 120.8(6) . . ?
C10 C11 C12 119.5(6) . . ?
F12 C12 C11 115.9(5) . . ?
F12 C12 C7 119.9(5) . . ?
C11 C12 C7 124.2(6) . . ?
C13 N1 C20 116.5(5) . . ?
C13 N1 Pt 121.6(4) . . ?
C20 N1 Pt 121.9(4) . . ?
C19 N2 C20 122.8(6) . . ?
C19 N2 H2 114(6) . . ?
C20 N2 H2 123(6) . . ?
N1 C13 C14 124.3(6) . . ?
N1 C13 H13 112(4) . . ?
C14 C13 H13 123(4) . . ?
C15 C14 C13 118.4(6) . . ?
C15 C14 H14 123(3) . . ?
C13 C14 H14 117(3) . . ?
C14 C15 C16 119.9(6) . . ?
C14 C15 H15 126(4) . . ?
C16 C15 H15 113(4) . . ?
C15 C16 C20 117.6(6) . . ?
C15 C16 C17 125.4(6) . . ?
C20 C16 C17 117.0(6) . . ?
C18 C17 C16 120.7(6) . . ?
C18 C17 H17 123(4) . . ?
C16 C17 H17 115(4) . . ?
C17 C18 C19 119.9(6) . . ?
C17 C18 H18 114(4) . . ?
C19 C18 H18 126(4) . . ?
N2 C19 C18 120.4(7) . . ?
N2 C19 H19 114(5) . . ?
C18 C19 H19 126(5) . . ?
N2 C20 N1 117.7(5) . . ?
N2 C20 C16 119.1(5) . . ?
N1 C20 C16 123.2(5) . . ?
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
Pt C1 1.994(6) . ?
Pt C7 1.996(6) . ?
Pt N1 2.099(5) . ?
Pt Cl 2.3781(16) . ?
C1 C2 1.373(8) . ?
C1 C6 1.385(8) . ?
C2 F2 1.361(7) . ?
C2 C3 1.372(8) . ?
C3 F3 1.346(7) . ?
C3 C4 1.361(10) . ?
C4 F4 1.340(7) . ?
C4 C5 1.366(9) . ?
C5 F5 1.347(7) . ?
C5 C6 1.367(9) . ?
C6 F6 1.361(7) . ?
C7 C8 1.361(8) . ?
C7 C12 1.380(8) . ?
C8 F8 1.346(7) . ?
C8 C9 1.376(9) . ?
C9 F9 1.356(8) . ?
C9 C10 1.368(11) . ?
C10 F10 1.348(7) . ?
C10 C11 1.353(10) . ?
C11 F11 1.354(8) . ?
C11 C12 1.363(9) . ?
C12 F12 1.362(7) . ?
N1 C13 1.312(7) . ?
N1 C20 1.363(7) . ?
N2 C19 1.320(8) . ?
N2 C20 1.346(7) . ?
N2 H2 0.76(7) . ?
C13 C14 1.408(9) . ?
C13 H13 0.92(7) . ?
C14 C15 1.354(10) . ?
C14 H14 1.14(6) . ?
C15 C16 1.389(9) . ?
C15 H15 0.91(7) . ?
C16 C20 1.404(8) . ?
C16 C17 1.416(9) . ?
C17 C18 1.346(11) . ?
C17 H17 0.95(7) . ?
C18 C19 1.362(11) . ?
C18 H18 0.93(7) . ?
C19 H19 0.85(7) . ?
