#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/20/4112035.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_4112035
loop_
_publ_author_name
'Fenbao Zhang'
'Christopher W. Kirby'
'Douglas W. Hairsine'
'Michael C. Jennings'
'Richard J. Puddephatt'
_publ_section_title
;
 Activation of C-H Bonds of Arenes: Selectivity and Reactivity in
 Bis(pyridyl) Platinum(II) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14196
_journal_page_last               14197
_journal_paper_doi               10.1021/ja055436z
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C37.5 H19 B Cl F15 N2 O4 Pt'
_chemical_formula_weight         1087.90
_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                 92.257(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6163(4)
_cell_length_b                   15.4527(6)
_cell_length_c                   22.3982(10)
_cell_measurement_temperature    150(2)
_cell_volume                     3671.6(3)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'phi/omega 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  0.077
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31649
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    4.017
_exptl_absorpt_correction_T_max  0.8244
_exptl_absorpt_correction_T_min  0.6336
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            orange/red
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.731
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         6386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0416
_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)+(0.0281P)²+12.5486P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                4699
_reflns_number_total             6386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja055436zsi20050817_031919_8.cif
_cod_data_source_block           complex_9a
_cod_original_formula_sum        'C37.50 H19 B Cl F15 N2 O4 Pt'
_cod_database_code               4112035
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
Pt Pt 0.61949(2) 0.628509(17) 0.296883(12) 0.02835(9) Uani 1 1 d .
N1 N 0.6870(4) 0.6254(3) 0.3800(2) 0.0288(12) Uani 1 1 d .
C2 C 0.8108(6) 0.6268(5) 0.3944(4) 0.0415(18) Uani 1 1 d .
H2A H 0.8688 0.6362 0.3639 0.050 Uiso 1 1 calc R
C3 C 0.8574(7) 0.6146(5) 0.4536(4) 0.046(2) Uani 1 1 d .
H3A H 0.9455 0.6171 0.4627 0.055 Uiso 1 1 calc R
C4 C 0.7759(7) 0.5995(6) 0.4977(4) 0.053(2) Uani 1 1 d .
H4A H 0.8060 0.5901 0.5377 0.063 Uiso 1 1 calc R
C5 C 0.6486(7) 0.5978(5) 0.4833(3) 0.0413(18) Uani 1 1 d .
H5A H 0.5901 0.5865 0.5133 0.050 Uiso 1 1 calc R
C6 C 0.6065(6) 0.6127(4) 0.4253(3) 0.0279(15) Uani 1 1 d .
C7 C 0.4656(6) 0.6199(5) 0.4131(3) 0.0334(16) Uani 1 1 d .
O8 O 0.3942(4) 0.5756(3) 0.4412(2) 0.0438(13) Uani 1 1 d .
C9 C 0.4151(6) 0.6926(4) 0.3738(3) 0.0297(15) Uani 1 1 d .
C10 C 0.3107(6) 0.7378(5) 0.3904(3) 0.0365(18) Uani 1 1 d .
H10A H 0.2651 0.7209 0.4241 0.044 Uiso 1 1 calc R
C11 C 0.2738(6) 0.8100(5) 0.3559(4) 0.0415(19) Uani 1 1 d .
H11A H 0.2020 0.8427 0.3660 0.050 Uiso 1 1 calc R
C12 C 0.3413(7) 0.8327(5) 0.3082(4) 0.0405(19) Uani 1 1 d .
H12A H 0.3195 0.8829 0.2856 0.049 Uiso 1 1 calc R
C13 C 0.4419(6) 0.7819(4) 0.2928(3) 0.0343(17) Uani 1 1 d .
H13A H 0.4866 0.7970 0.2584 0.041 Uiso 1 1 calc R
N14 N 0.4791(5) 0.7122(3) 0.3244(3) 0.0307(13) Uani 1 1 d .
C21 C 0.7569(6) 0.5495(4) 0.2710(3) 0.0320(16) Uani 1 1 d .
C22 C 0.8286(6) 0.5673(4) 0.2211(3) 0.0295(16) Uani 1 1 d .
C23 C 0.9255(6) 0.5148(5) 0.2043(3) 0.0375(18) Uani 1 1 d .
H23A H 0.9711 0.5287 0.1699 0.045 Uiso 1 1 calc R
C24 C 0.9571(6) 0.4410(5) 0.2376(4) 0.0396(18) Uani 1 1 d .
C25 C 0.8910(6) 0.4207(5) 0.2871(3) 0.0377(18) Uani 1 1 d .
H25A H 0.9112 0.3708 0.3103 0.045 Uiso 1 1 calc R
C26 C 0.7938(6) 0.4753(4) 0.3023(3) 0.0338(17) Uani 1 1 d .
H26A H 0.7488 0.4610 0.3368 0.041 Uiso 1 1 calc R
O27 O 0.7959(4) 0.6428(3) 0.1905(2) 0.0346(12) Uani 1 1 d .
C28 C 0.8679(6) 0.6663(5) 0.1402(3) 0.0436(19) Uani 1 1 d .
H28A H 0.8349 0.7204 0.1230 0.065 Uiso 1 1 calc R
H28B H 0.8617 0.6204 0.1101 0.065 Uiso 1 1 calc R
H28C H 0.9563 0.6743 0.1532 0.065 Uiso 1 1 calc R
O29 O 1.0545(4) 0.3946(4) 0.2163(3) 0.0556(16) Uani 1 1 d .
C30 C 1.0982(7) 0.3217(5) 0.2496(4) 0.052(2) Uani 1 1 d .
H30A H 1.1671 0.2940 0.2289 0.077 Uiso 1 1 calc R
H30B H 1.0290 0.2804 0.2535 0.077 Uiso 1 1 calc R
H30C H 1.1288 0.3404 0.2894 0.077 Uiso 1 1 calc R
O31 O 0.5451(4) 0.6310(3) 0.21084(19) 0.0296(10) Uani 1 1 d .
H31A H 0.6002 0.6575 0.1838 0.035 Uiso 1 1 calc R
B32 B 0.4224(7) 0.6005(5) 0.1800(4) 0.0280(18) Uani 1 1 d .
C41 C 0.3646(4) 0.6799(2) 0.1336(2) 0.0315(16) Uani 1 1 d G
C42 C 0.2467(4) 0.6649(2) 0.1063(2) 0.0362(17) Uani 1 1 d G
C43 C 0.1884(3) 0.7291(3) 0.0716(2) 0.044(2) Uani 1 1 d G
C44 C 0.2478(4) 0.8083(3) 0.0642(2) 0.0414(19) Uani 1 1 d G
C45 C 0.3657(4) 0.8233(2) 0.0915(2) 0.0382(18) Uani 1 1 d G
C46 C 0.4240(3) 0.7591(3) 0.1262(2) 0.0340(17) Uani 1 1 d G
F42 F 0.1850(3) 0.5928(3) 0.11258(19) 0.0473(11) Uani 1 1 d .
F43 F 0.0737(4) 0.7167(3) 0.0464(2) 0.0714(16) Uani 1 1 d .
F44 F 0.1887(4) 0.8720(3) 0.0317(2) 0.0656(14) Uani 1 1 d .
F45 F 0.4217(4) 0.8995(3) 0.0841(2) 0.0509(12) Uani 1 1 d .
F46 F 0.5370(3) 0.7774(3) 0.14820(19) 0.0447(11) Uani 1 1 d .
C51 C 0.3277(3) 0.5776(3) 0.23632(16) 0.0279(15) Uani 1 1 d G
C52 C 0.3575(3) 0.5053(2) 0.27096(19) 0.0303(16) Uani 1 1 d G
C53 C 0.2854(4) 0.4846(2) 0.31942(18) 0.0295(16) Uani 1 1 d G
C54 C 0.1834(4) 0.5363(3) 0.33325(16) 0.0308(16) Uani 1 1 d G
C55 C 0.1536(3) 0.6087(2) 0.29861(19) 0.0325(17) Uani 1 1 d G
C56 C 0.2257(3) 0.6293(2) 0.25014(17) 0.0271(14) Uani 1 1 d G
F52 F 0.4519(3) 0.4542(2) 0.26007(18) 0.0372(10) Uani 1 1 d .
F53 F 0.3138(3) 0.4168(2) 0.35373(18) 0.0404(10) Uani 1 1 d .
F54 F 0.1148(3) 0.5173(3) 0.38139(18) 0.0410(10) Uani 1 1 d .
F55 F 0.0575(3) 0.6587(2) 0.31339(18) 0.0395(10) Uani 1 1 d .
F56 F 0.1904(3) 0.6996(2) 0.22125(17) 0.0345(9) Uani 1 1 d .
C61 C 0.4516(4) 0.5167(3) 0.13308(18) 0.0314(16) Uani 1 1 d G
C62 C 0.5527(4) 0.5260(3) 0.0960(2) 0.0347(17) Uani 1 1 d G
C63 C 0.5776(4) 0.4623(3) 0.05430(19) 0.045(2) Uani 1 1 d G
C64 C 0.5015(5) 0.3892(3) 0.04966(19) 0.049(2) Uani 1 1 d G
C65 C 0.4004(5) 0.3799(2) 0.0867(2) 0.048(2) Uani 1 1 d G
C66 C 0.3755(4) 0.4436(3) 0.1284(2) 0.0380(18) Uani 1 1 d G
F62 F 0.6228(3) 0.5954(3) 0.09624(18) 0.0456(11) Uani 1 1 d .
F63 F 0.6761(4) 0.4697(3) 0.0194(2) 0.0642(14) Uani 1 1 d .
F64 F 0.5258(5) 0.3269(3) 0.0088(2) 0.0680(15) Uani 1 1 d .
F65 F 0.3265(5) 0.3108(3) 0.0802(2) 0.0713(15) Uani 1 1 d .
F66 F 0.2785(4) 0.4303(3) 0.1610(2) 0.0534(12) Uani 1 1 d .
C71 C 1.0607(19) 0.4166(11) 0.0488(12) 0.102(9) Uani 0.50 1 d P
H71A H 1.1081 0.4504 0.0798 0.153 Uiso 0.50 1 calc PR
H71B H 1.1180 0.4076 0.0156 0.153 Uiso 0.50 1 calc PR
Cl72 Cl 1.0272(7) 0.3067(6) 0.0819(3) 0.128(3) Uani 0.50 1 d P
Cl73 Cl 0.9674(9) 0.4652(5) 0.0285(5) 0.174(5) Uani 0.50 1 d P
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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 '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'
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_3
N1 Pt C21 90.9(2) .
N1 Pt O31 178.71(19) .
C21 Pt O31 89.9(2) .
N1 Pt N14 88.5(2) .
C21 Pt N14 179.0(2) .
O31 Pt N14 90.71(19) .
C2 N1 C6 117.3(6) .
C2 N1 Pt 123.0(5) .
C6 N1 Pt 119.4(4) .
N1 C2 C3 122.0(7) .
C4 C3 C2 119.7(7) .
C3 C4 C5 118.7(8) .
C6 C5 C4 119.9(7) .
N1 C6 C5 122.3(6) .
N1 C6 C7 119.9(6) .
C5 C6 C7 117.7(6) .
O8 C7 C9 120.4(6) .
O8 C7 C6 119.8(6) .
C9 C7 C6 119.0(6) .
N14 C9 C10 122.9(6) .
N14 C9 C7 117.7(6) .
C10 C9 C7 119.3(6) .
C9 C10 C11 117.7(7) .
C12 C11 C10 119.7(7) .
C11 C12 C13 119.1(7) .
N14 C13 C12 122.8(7) .
C13 N14 C9 117.6(6) .
C13 N14 Pt 122.9(5) .
C9 N14 Pt 119.3(4) .
C26 C21 C22 114.3(6) .
C26 C21 Pt 123.3(5) .
C22 C21 Pt 122.3(5) .
C23 C22 O27 122.3(6) .
C23 C22 C21 122.6(6) .
O27 C22 C21 115.1(6) .
C22 C23 C24 120.1(7) .
O29 C24 C25 125.7(7) .
O29 C24 C23 114.3(7) .
C25 C24 C23 119.9(7) .
C24 C25 C26 118.0(7) .
C25 C26 C21 125.1(7) .
C22 O27 C28 118.1(5) .
C24 O29 C30 118.1(6) .
B32 O31 Pt 135.1(4) .
O31 B32 C51 104.6(5) .
O31 B32 C61 110.0(5) .
C51 B32 C61 115.6(5) .
O31 B32 C41 109.4(5) .
C51 B32 C41 113.4(5) .
C61 B32 C41 103.9(5) .
C42 C41 C46 120.0 .
C42 C41 B32 116.3(3) .
C46 C41 B32 123.5(3) .
F42 C42 C41 122.9(3) .
F42 C42 C43 117.1(3) .
C41 C42 C43 120.0 .
F43 C43 C42 120.8(4) .
F43 C43 C44 119.1(4) .
C42 C43 C44 120.0 .
F44 C44 C43 119.9(4) .
F44 C44 C45 120.1(4) .
C43 C44 C45 120.0 .
F45 C45 C44 119.4(4) .
F45 C45 C46 120.6(4) .
C44 C45 C46 120.0 .
F46 C46 C45 116.0(3) .
F46 C46 C41 124.0(3) .
C45 C46 C41 120.0 .
C52 C51 C56 120.0 .
C52 C51 B32 117.3(3) .
C56 C51 B32 122.7(3) .
F52 C52 C53 117.2(3) .
F52 C52 C51 122.8(3) .
C53 C52 C51 120.0 .
F53 C53 C52 120.9(3) .
F53 C53 C54 119.1(3) .
C52 C53 C54 120.0 .
F54 C54 C53 120.0(3) .
F54 C54 C55 120.0(3) .
C53 C54 C55 120.0 .
F55 C55 C56 120.8(3) .
F55 C55 C54 119.2(3) .
C56 C55 C54 120.0 .
F56 C56 C55 114.8(3) .
F56 C56 C51 125.2(3) .
C55 C56 C51 120.0 .
C62 C61 C66 120.0 .
C62 C61 B32 117.0(4) .
C66 C61 B32 122.9(4) .
F62 C62 C61 122.4(4) .
F62 C62 C63 117.4(4) .
C61 C62 C63 120.0 .
F63 C63 C62 120.5(4) .
F63 C63 C64 119.5(4) .
C62 C63 C64 120.0 .
F64 C64 C65 120.0(4) .
F64 C64 C63 120.0(4) .
C65 C64 C63 120.0 .
F65 C65 C64 118.9(4) .
F65 C65 C66 121.0(4) .
C64 C65 C66 120.0 .
F66 C66 C65 116.1(4) .
F66 C66 C61 123.9(4) .
C65 C66 C61 120.0 .
Cl73 C71 Cl72 120.0(14) .
C71 Cl73 Cl73 106.2(15) 3_765
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt N1 1.969(5) .
Pt C21 2.005(7) .
Pt O31 2.054(4) .
Pt N14 2.085(5) .
N1 C2 1.341(8) .
N1 C6 1.367(8) .
C2 C3 1.409(10) .
C3 C4 1.358(11) .
C4 C5 1.376(10) .
C5 C6 1.376(9) .
C6 C7 1.514(9) .
C7 O8 1.214(8) .
C7 C9 1.513(9) .
C9 N14 1.355(8) .
C9 C10 1.374(9) .
C10 C11 1.403(10) .
C11 C12 1.356(10) .
C12 C13 1.380(10) .
C13 N14 1.338(8) .
C21 C26 1.392(9) .
C21 C22 1.403(9) .
C22 C23 1.375(9) .
C22 O27 1.391(8) .
C23 C24 1.396(10) .
C24 O29 1.360(8) .
C24 C25 1.371(10) .
C25 C26 1.386(9) .
O27 C28 1.432(8) .
O29 C30 1.419(9) .
O31 B32 1.525(8) .
B32 C51 1.680(9) .
B32 C61 1.704(9) .
B32 C41 1.708(8) .
C41 C42 1.3900 .
C41 C46 1.3900 .
C42 F42 1.302(5) .
C42 C43 1.3900 .
C43 F43 1.335(5) .
C43 C44 1.3900 .
C44 F44 1.363(5) .
C44 C45 1.3900 .
C45 F45 1.333(5) .
C45 C46 1.3900 .
C46 F46 1.310(5) .
C51 C52 1.3900 .
C51 C56 1.3900 .
C52 F52 1.306(4) .
C52 C53 1.3900 .
C53 F53 1.327(5) .
C53 C54 1.3900 .
C54 F54 1.357(5) .
C54 C55 1.3900 .
C55 F55 1.333(4) .
C55 C56 1.3900 .
C56 F56 1.312(4) .
C61 C62 1.3900 .
C61 C66 1.3900 .
C62 F62 1.305(5) .
C62 C63 1.3900 .
C63 F63 1.334(5) .
C63 C64 1.3900 .
C64 F64 1.360(5) .
C64 C65 1.3900 .
C65 F65 1.330(5) .
C65 C66 1.3900 .
C66 F66 1.302(5) .
C71 Cl73 1.31(2) .
C71 Cl72 1.89(2) .
Cl73 Cl73 1.83(2) 3_765
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O31 H31A O27 0.95 2.09 2.725(6) 122.9
O31 H31A F46 0.95 2.12 2.662(6) 115.0
O31 H31A F62 0.95 2.21 2.782(6) 118.1
