#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:27:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179378 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/75/4327576.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_4327576
loop_
_publ_author_name
'Joel T. Mague'
'Jamin L. Krinsky'
_publ_section_title
;
 Synthetic and Structural Studies of the Coordination Behavior of
 2-Pyridylbis(diphenylphosphino)methane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1962
_journal_page_last               1971
_journal_paper_doi               10.1021/ic001266+
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '(((C6 H5)2 P)2 C (C5 H4 N))((C6 H5)3)P H Pt'
_chemical_formula_sum            'C48 H40 N P3 Pt'
_chemical_formula_weight         918.81
_chemical_name_systematic
; 
 Hydrido(η²-(2-pyridylbis(diphenylphosphino)methanido))triphenylphosphine 
 platinum(II)
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.975(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0878(11)
_cell_length_b                   12.8836(9)
_cell_length_c                   18.4228(17)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.23
_cell_measurement_theta_min      21.52
_cell_volume                     3952.6(6)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1987)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS, 1997)'
_computing_publication_material  'SHELXTL (Bruker AXS, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       'θ/2θ 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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7270
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.707
_exptl_absorpt_correction_T_max  0.7241
_exptl_absorpt_correction_T_min  0.4426
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ψ scan (Phillips, et al., 1968)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.734
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0427P)²+1.5430P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                5069
_reflns_number_total             7031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0012662B_10.cif
_cod_data_source_block           14
_cod_original_cell_volume        3952.6(5)
_cod_database_code               4327576
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 0.266416(11) 0.123719(14) 0.864997(10) 0.02835(7) Uani 1 1 d .
P1 P 0.30925(8) 0.29195(10) 0.89276(7) 0.0305(3) Uani 1 1 d .
P2 P 0.24670(7) 0.05765(9) 0.97373(7) 0.0273(3) Uani 1 1 d .
P3 P 0.22280(7) -0.04543(9) 0.84027(7) 0.0279(3) Uani 1 1 d .
N N 0.1716(3) -0.2406(3) 0.9140(3) 0.0457(11) Uani 1 1 d .
C1 C 0.2128(3) -0.0633(4) 0.9299(3) 0.0311(11) Uani 1 1 d .
C2 C 0.1903(3) -0.1552(4) 0.9609(3) 0.0338(11) Uani 1 1 d .
C3 C 0.1867(3) -0.1575(4) 1.0353(3) 0.0416(13) Uani 1 1 d .
H3 H 0.2006 -0.0990 1.0675 0.046 Uiso 1 1 calc R
C4 C 0.1625(3) -0.2466(5) 1.0606(4) 0.0499(15) Uani 1 1 d .
H4 H 0.1595 -0.2489 1.1098 0.055 Uiso 1 1 calc R
C5 C 0.1429(4) -0.3322(5) 1.0124(4) 0.0568(17) Uani 1 1 d .
H5 H 0.1259 -0.3933 1.0279 0.063 Uiso 1 1 calc R
C6 C 0.1490(4) -0.3250(4) 0.9415(4) 0.0575(17) Uani 1 1 d .
H6 H 0.1364 -0.3838 0.9096 0.063 Uiso 1 1 calc R
C7 C 0.2916(3) -0.1409(4) 0.8278(3) 0.0317(11) Uani 1 1 d .
C8 C 0.2920(3) -0.1602(4) 0.7547(3) 0.0394(12) Uani 1 1 d .
H8 H 0.2586 -0.1227 0.7111 0.043 Uiso 1 1 calc R
C9 C 0.3434(4) -0.2374(5) 0.7462(4) 0.0543(16) Uani 1 1 d .
H9 H 0.3430 -0.2525 0.6967 0.060 Uiso 1 1 calc R
C10 C 0.3939(4) -0.2899(5) 0.8112(4) 0.0589(17) Uani 1 1 d .
H10 H 0.4281 -0.3403 0.8057 0.065 Uiso 1 1 calc R
C11 C 0.3946(3) -0.2690(5) 0.8838(4) 0.0554(16) Uani 1 1 d .
H11 H 0.4299 -0.3043 0.9276 0.061 Uiso 1 1 calc R
C12 C 0.3433(3) -0.1960(4) 0.8927(3) 0.0426(13) Uani 1 1 d .
H12 H 0.3431 -0.1834 0.9424 0.047 Uiso 1 1 calc R
C13 C 0.1314(3) -0.0643(4) 0.7513(3) 0.0335(11) Uani 1 1 d .
C14 C 0.0996(4) 0.0165(5) 0.7006(4) 0.0619(18) Uani 1 1 d .
H14 H 0.1243 0.0812 0.7125 0.068 Uiso 1 1 calc R
C15 C 0.0325(5) 0.0049(7) 0.6329(4) 0.085(2) Uani 1 1 d .
H15 H 0.0123 0.0614 0.5996 0.093 Uiso 1 1 calc R
C16 C -0.0045(4) -0.0876(7) 0.6142(4) 0.078(2) Uani 1 1 d .
H16 H -0.0497 -0.0959 0.5678 0.086 Uiso 1 1 calc R
C17 C 0.0254(4) -0.1692(6) 0.6646(4) 0.071(2) Uani 1 1 d .
H17 H -0.0006 -0.2330 0.6527 0.078 Uiso 1 1 calc R
C18 C 0.0932(4) -0.1589(5) 0.7324(4) 0.0503(15) Uani 1 1 d .
H18 H 0.1132 -0.2157 0.7655 0.055 Uiso 1 1 calc R
C19 C 0.3378(3) 0.0462(4) 1.0628(3) 0.0327(11) Uani 1 1 d .
C20 C 0.3398(4) 0.0431(5) 1.1391(3) 0.0479(14) Uani 1 1 d .
H20 H 0.2920 0.0433 1.1469 0.053 Uiso 1 1 calc R
C21 C 0.4129(5) 0.0398(5) 1.2036(4) 0.069(2) Uani 1 1 d .
H21 H 0.4138 0.0402 1.2545 0.075 Uiso 1 1 calc R
C22 C 0.4834(4) 0.0360(5) 1.1926(4) 0.0650(19) Uani 1 1 d .
H22 H 0.5319 0.0329 1.2361 0.071 Uiso 1 1 calc R
C23 C 0.4833(4) 0.0366(4) 1.1188(4) 0.0569(17) Uani 1 1 d .
H23 H 0.5314 0.0345 1.1117 0.063 Uiso 1 1 calc R
C24 C 0.4104(3) 0.0405(4) 1.0540(3) 0.0439(13) Uani 1 1 d .
H24 H 0.4103 0.0391 1.0035 0.048 Uiso 1 1 calc R
C25 C 0.1722(3) 0.1165(4) 1.0053(3) 0.0315(10) Uani 1 1 d .
C26 C 0.0933(3) 0.0816(4) 0.9712(3) 0.0426(13) Uani 1 1 d .
H26 H 0.0797 0.0281 0.9343 0.047 Uiso 1 1 calc R
C27 C 0.0352(3) 0.1267(5) 0.9922(4) 0.0549(15) Uani 1 1 d .
H27 H -0.0175 0.1034 0.9693 0.060 Uiso 1 1 calc R
C28 C 0.0545(4) 0.2060(5) 1.0469(4) 0.0617(18) Uani 1 1 d .
H28 H 0.0153 0.2349 1.0616 0.068 Uiso 1 1 calc R
C29 C 0.1319(4) 0.2415(5) 1.0791(4) 0.0641(19) Uani 1 1 d .
H29 H 0.1447 0.2964 1.1147 0.071 Uiso 1 1 calc R
C30 C 0.1911(3) 0.1973(5) 1.0596(3) 0.0470(14) Uani 1 1 d .
H30 H 0.2436 0.2215 1.0827 0.052 Uiso 1 1 calc R
C31 C 0.4092(3) 0.3129(4) 0.8931(3) 0.0339(11) Uani 1 1 d .
C32 C 0.4506(3) 0.4058(4) 0.9176(3) 0.0372(12) Uani 1 1 d .
H32 H 0.4265 0.4608 0.9328 0.041 Uiso 1 1 calc R
C33 C 0.5275(4) 0.4170(5) 0.9196(3) 0.0469(14) Uani 1 1 d .
H33 H 0.5544 0.4797 0.9357 0.052 Uiso 1 1 calc R
C34 C 0.5640(4) 0.3371(5) 0.8983(4) 0.0562(17) Uani 1 1 d .
H34 H 0.6155 0.3456 0.8994 0.062 Uiso 1 1 calc R
C35 C 0.5250(4) 0.2440(5) 0.8752(4) 0.0643(19) Uani 1 1 d .
H35 H 0.5506 0.1888 0.8621 0.071 Uiso 1 1 calc R
C36 C 0.4472(4) 0.2322(4) 0.8714(4) 0.0504(15) Uani 1 1 d .
H36 H 0.4203 0.1697 0.8541 0.055 Uiso 1 1 calc R
C37 C 0.2394(3) 0.3842(4) 0.8230(3) 0.0378(12) Uani 1 1 d .
C38 C 0.1619(5) 0.3547(5) 0.7845(4) 0.078(2) Uani 1 1 d .
H38 H 0.1468 0.2872 0.7903 0.085 Uiso 1 1 calc R
C39 C 0.1048(5) 0.4234(7) 0.7368(5) 0.096(3) Uani 1 1 d .
H39 H 0.0513 0.4032 0.7126 0.106 Uiso 1 1 calc R
C40 C 0.1273(5) 0.5199(6) 0.7256(4) 0.078(2) Uani 1 1 d .
H40 H 0.0894 0.5658 0.6926 0.086 Uiso 1 1 calc R
C41 C 0.2027(5) 0.5494(6) 0.7611(6) 0.097(3) Uani 1 1 d .
H41 H 0.2179 0.6161 0.7532 0.107 Uiso 1 1 calc R
C42 C 0.2593(4) 0.4809(5) 0.8102(5) 0.081(2) Uani 1 1 d .
H42 H 0.3124 0.5025 0.8350 0.089 Uiso 1 1 calc R
C43 C 0.3215(3) 0.3427(4) 0.9896(3) 0.0315(11) Uani 1 1 d .
C44 C 0.3821(3) 0.3027(4) 1.0566(3) 0.0370(12) Uani 1 1 d .
H44 H 0.4183 0.2552 1.0510 0.041 Uiso 1 1 calc R
C45 C 0.3896(3) 0.3321(5) 1.1307(3) 0.0461(14) Uani 1 1 d .
H45 H 0.4300 0.3034 1.1747 0.051 Uiso 1 1 calc R
C46 C 0.3377(4) 0.4036(5) 1.1403(4) 0.0531(16) Uani 1 1 d .
H46 H 0.3428 0.4233 1.1906 0.058 Uiso 1 1 calc R
C47 C 0.2788(4) 0.4456(5) 1.0754(4) 0.0599(17) Uani 1 1 d .
H47 H 0.2443 0.4948 1.0819 0.066 Uiso 1 1 calc R
C48 C 0.2695(3) 0.4160(5) 0.9998(3) 0.0485(14) Uani 1 1 d .
H48 H 0.2288 0.4449 0.9562 0.053 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'
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'
P P 0.1023 0.0942 '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_publ_flag
P1 Pt P3 178.43(4) y
P1 Pt P2 107.80(4) y
P3 Pt P2 70.64(4) y
C31 P1 C43 101.6(2) ?
C31 P1 C37 108.4(2) ?
C43 P1 C37 103.8(2) ?
C31 P1 Pt 112.87(17) ?
C43 P1 Pt 117.22(16) ?
C37 P1 Pt 111.98(17) ?
C1 P2 C19 112.0(2) ?
C1 P2 C25 110.3(2) ?
C19 P2 C25 105.5(2) ?
C1 P2 Pt 94.12(15) ?
C19 P2 Pt 114.56(17) ?
C25 P2 Pt 120.11(16) ?
C1 P2 P3 39.94(15) ?
C19 P2 P3 123.50(17) ?
C25 P2 P3 128.58(16) ?
Pt P2 P3 54.22(4) ?
C1 P3 C7 110.9(2) ?
C1 P3 C13 116.0(2) ?
C7 P3 C13 102.7(2) ?
C1 P3 Pt 95.25(16) ?
C7 P3 Pt 117.70(15) ?
C13 P3 Pt 114.96(17) ?
C1 P3 P2 40.14(16) ?
C7 P3 P2 125.14(16) ?
C13 P3 P2 130.74(16) ?
Pt P3 P2 55.15(4) ?
C6 N C2 117.2(5) ?
C2 C1 P3 129.3(4) y
C2 C1 P2 130.5(4) y
P3 C1 P2 99.9(2) y
N C2 C3 120.8(5) ?
N C2 C1 116.9(4) ?
C3 C2 C1 122.4(5) ?
C4 C3 C2 119.5(5) ?
C5 C4 C3 119.3(6) ?
C6 C5 C4 118.0(6) ?
N C6 C5 125.1(6) ?
C8 C7 C12 119.5(5) ?
C8 C7 P3 120.6(4) ?
C12 C7 P3 119.8(4) ?
C7 C8 C9 119.5(5) ?
C10 C9 C8 119.6(6) ?
C11 C10 C9 120.7(6) ?
C10 C11 C12 120.4(6) ?
C11 C12 C7 120.3(5) ?
C14 C13 C18 117.8(5) ?
C14 C13 P3 120.1(4) ?
C18 C13 P3 122.1(4) ?
C15 C14 C13 121.8(7) ?
C16 C15 C14 120.5(7) ?
C15 C16 C17 118.8(6) ?
C16 C17 C18 121.4(7) ?
C17 C18 C13 119.8(6) ?
C24 C19 C20 117.7(5) ?
C24 C19 P2 117.7(4) ?
C20 C19 P2 124.6(4) ?
C21 C20 C19 120.3(6) ?
C22 C21 C20 120.3(6) ?
C23 C22 C21 120.7(6) ?
C22 C23 C24 119.2(6) ?
C19 C24 C23 121.7(6) ?
C30 C25 C26 119.2(5) ?
C30 C25 P2 122.4(4) ?
C26 C25 P2 118.4(4) ?
C27 C26 C25 119.7(5) ?
C28 C27 C26 120.9(6) ?
C29 C28 C27 119.2(5) ?
C28 C29 C30 121.0(6) ?
C29 C30 C25 120.0(5) ?
C36 C31 C32 118.3(5) ?
C36 C31 P1 119.3(4) ?
C32 C31 P1 122.3(4) ?
C33 C32 C31 120.4(5) ?
C34 C33 C32 120.6(5) ?
C33 C34 C35 120.1(5) ?
C34 C35 C36 120.0(6) ?
C31 C36 C35 120.6(5) ?
C42 C37 C38 117.5(6) ?
C42 C37 P1 124.3(5) ?
C38 C37 P1 118.2(4) ?
C37 C38 C39 121.1(7) ?
C40 C39 C38 119.4(8) ?
C41 C40 C39 120.5(7) ?
C40 C41 C42 119.8(7) ?
C37 C42 C41 121.7(7) ?
C44 C43 C48 118.0(5) ?
C44 C43 P1 119.1(4) ?
C48 C43 P1 122.8(4) ?
C45 C44 C43 121.2(5) ?
C44 C45 C46 120.4(5) ?
C47 C46 C45 119.4(5) ?
C46 C47 C48 121.2(6) ?
C47 C48 C43 119.8(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pt P1 2.2913(12) y
Pt P3 2.3019(12) y
Pt P2 2.3285(12) y
P1 C31 1.826(5) ?
P1 C43 1.830(5) ?
P1 C37 1.842(5) ?
P2 C1 1.752(5) y
P2 C19 1.822(5) y
P2 C25 1.828(5) y
P2 P3 2.6770(16) ?
P3 C1 1.745(4) y
P3 C7 1.827(5) y
P3 C13 1.833(5) y
N C6 1.330(7) ?
N C2 1.358(6) ?
C1 C2 1.441(7) y
C2 C3 1.397(7) ?
C3 C4 1.373(7) ?
C4 C5 1.372(9) ?
C5 C6 1.357(9) ?
C7 C8 1.373(7) ?
C7 C12 1.390(7) ?
C8 C9 1.412(8) ?
C9 C10 1.368(9) ?
C10 C11 1.358(9) ?
C11 C12 1.376(8) ?
C13 C14 1.367(8) ?
C13 C18 1.378(8) ?
C14 C15 1.368(9) ?
C15 C16 1.344(11) ?
C16 C17 1.367(11) ?
C17 C18 1.373(9) ?
C19 C24 1.385(7) ?
C19 C20 1.393(7) ?
C20 C21 1.392(8) ?
C21 C22 1.369(10) ?
C22 C23 1.359(9) ?
C23 C24 1.392(8) ?
C25 C30 1.390(7) ?
C25 C26 1.391(7) ?
C26 C27 1.382(8) ?
C27 C28 1.379(9) ?
C28 C29 1.368(9) ?
C29 C30 1.378(8) ?
C31 C36 1.388(7) ?
C31 C32 1.391(7) ?
C32 C33 1.384(7) ?
C33 C34 1.362(9) ?
C34 C35 1.372(8) ?
C35 C36 1.389(8) ?
C37 C42 1.343(8) ?
C37 C38 1.355(9) ?
C38 C39 1.383(10) ?
C39 C40 1.349(11) ?
C40 C41 1.317(10) ?
C41 C42 1.387(9) ?
C43 C44 1.391(7) ?
C43 C48 1.397(7) ?
C44 C45 1.372(7) ?
C45 C46 1.375(8) ?
C46 C47 1.365(8) ?
C47 C48 1.389(8) ?
