#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:46:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179127 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/89/4308952.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_4308952
loop_
_publ_author_name
'Alvaro Díez'
'Juan Forniés'
'Ana García'
'Elena Lalinde'
'M. Teresa Moreno'
_publ_section_title
;
Synthesis, Structural Characterization, and Photophysical Properties of
Palladium and Platinum(II) Complexes Containing 7,8-Benzoquinolinate and
Various Phosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2443
_journal_page_last               2453
_journal_paper_doi               10.1021/ic048272g
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C50 H36 N2 P2 Pt2'
_chemical_formula_weight         1116.93
_chemical_name_common            'jbm32: adsp'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                103.6040(10)
_cell_angle_beta                 103.9800(10)
_cell_angle_gamma                100.4650(10)
_cell_formula_units_Z            1
_cell_length_a                   8.9636(2)
_cell_length_b                   10.7454(2)
_cell_length_c                   10.8301(3)
_cell_measurement_reflns_used    4227
_cell_measurement_temperature    173.0(10)
_cell_volume                     951.87(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173.0(10)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0395522
_diffrn_orient_matrix_UB_12      0.0704553
_diffrn_orient_matrix_UB_13      -0.0339997
_diffrn_orient_matrix_UB_21      -0.0214313
_diffrn_orient_matrix_UB_22      0.0360783
_diffrn_orient_matrix_UB_23      0.0860872
_diffrn_orient_matrix_UB_31      0.1099838
_diffrn_orient_matrix_UB_32      0.0594004
_diffrn_orient_matrix_UB_33      0.0365261
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4513
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         2.4
_exptl_absorpt_coefficient_mu    7.465
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       neddle
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.864
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0172P)²+1.9339P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.048
_reflns_number_gt                4290
_reflns_number_total             4513
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048272gsi20041209_011236_4.cif
_cod_data_source_block           for_complex8
_cod_database_code               4308952
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Pt1 Pt 0.070991(13) 0.857392(11) 0.019718(11) 0.01870(4) Uani 1 1 d . . .
P1 P -0.00977(9) 1.03008(8) 0.13401(8) 0.01794(15) Uani 1 1 d . . .
N1 N 0.1066(3) 0.7500(3) 0.1576(3) 0.0284(6) Uani 1 1 d . . .
C1 C 0.1682(3) 0.7151(3) -0.0775(3) 0.0179(6) Uani 1 1 d . . .
C2 C 0.2203(4) 0.7078(3) -0.1870(4) 0.0294(7) Uani 1 1 d . . .
H2 H 0.2086 0.7712 -0.2317 0.035 Uiso 1 1 calc R . .
C3 C 0.2907(4) 0.6076(4) -0.2339(4) 0.0342(8) Uani 1 1 d . . .
H3 H 0.3265 0.6061 -0.3079 0.041 Uiso 1 1 calc R . .
C4 C 0.3075(4) 0.5109(4) -0.1709(4) 0.0345(8) Uani 1 1 d . . .
H4 H 0.3495 0.4421 -0.2048 0.041 Uiso 1 1 calc R . .
C5 C 0.2611(4) 0.5172(3) -0.0564(4) 0.0279(7) Uani 1 1 d . . .
C6 C 0.1949(4) 0.6219(3) -0.0102(3) 0.0230(6) Uani 1 1 d . . .
C7 C 0.2815(4) 0.4255(3) 0.0210(4) 0.0345(8) Uani 1 1 d . . .
H7 H 0.3209 0.3538 -0.0098 0.041 Uiso 1 1 calc R . .
C8 C 0.2451(4) 0.4409(3) 0.1362(4) 0.0327(8) Uani 1 1 d . . .
H8 H 0.2587 0.3791 0.1827 0.039 Uiso 1 1 calc R . .
C9 C 0.1858(4) 0.5506(3) 0.1886(4) 0.0269(7) Uani 1 1 d . . .
C10 C 0.1602(3) 0.6398(3) 0.1136(3) 0.0230(6) Uani 1 1 d . . .
C11 C 0.1518(4) 0.5749(4) 0.3104(4) 0.0344(8) Uani 1 1 d . . .
H11 H 0.164 0.5166 0.3612 0.041 Uiso 1 1 calc R . .
C12 C 0.1004(5) 0.6851(4) 0.3544(4) 0.0377(9) Uani 1 1 d . . .
H12 H 0.0796 0.7023 0.436 0.045 Uiso 1 1 calc R . .
C13 C 0.0791(5) 0.7718(4) 0.2773(4) 0.0348(8) Uani 1 1 d . . .
H13 H 0.0451 0.8465 0.3093 0.042 Uiso 1 1 calc R . .
C14 C 0.1578(4) 1.1359(3) 0.2772(3) 0.0213(6) Uani 1 1 d . . .
C15 C 0.3098(4) 1.1166(4) 0.2883(4) 0.0287(7) Uani 1 1 d . . .
H15 H 0.3236 1.0467 0.2264 0.034 Uiso 1 1 calc R . .
C16 C 0.4412(4) 1.2005(4) 0.3906(4) 0.0353(8) Uani 1 1 d . . .
H16 H 0.5418 1.1867 0.3963 0.042 Uiso 1 1 calc R . .
C17 C 0.4220(4) 1.3042(4) 0.4835(4) 0.0381(9) Uani 1 1 d . . .
H17 H 0.5094 1.3609 0.5515 0.046 Uiso 1 1 calc R . .
C18 C 0.2718(5) 1.3231(3) 0.4744(4) 0.0348(8) Uani 1 1 d . . .
H18 H 0.2582 1.3915 0.5379 0.042 Uiso 1 1 calc R . .
C19 C 0.1414(4) 1.2411(3) 0.3716(3) 0.0284(7) Uani 1 1 d . . .
H19 H 0.0416 1.2567 0.3656 0.034 Uiso 1 1 calc R . .
C20 C -0.1713(4) 0.9843(3) 0.2031(3) 0.0210(6) Uani 1 1 d . . .
C21 C -0.1539(4) 0.9954(3) 0.3368(3) 0.0257(7) Uani 1 1 d . . .
H21 H -0.0541 1.0326 0.3989 0.031 Uiso 1 1 calc R . .
C22 C -0.2834(4) 0.9518(4) 0.3790(4) 0.0327(8) Uani 1 1 d . . .
H22 H -0.2705 0.9613 0.4689 0.039 Uiso 1 1 calc R . .
C24 C -0.4515(4) 0.8852(4) 0.1537(4) 0.0347(8) Uani 1 1 d . . .
H24 H -0.5519 0.85 0.0922 0.042 Uiso 1 1 calc R . .
C23 C -0.4324(4) 0.8939(4) 0.2862(4) 0.0360(8) Uani 1 1 d . . .
H23 H -0.5186 0.8612 0.3132 0.043 Uiso 1 1 calc R . .
C25 C -0.3225(4) 0.9286(3) 0.1119(4) 0.0288(7) Uani 1 1 d . . .
H25 H -0.3367 0.9205 0.0222 0.035 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 0 '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'
P P 0.1023 0.0942 '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 0.006 '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
N1 Pt1 C1 80.01(12) . . ?
N1 Pt1 P1 175.27(8) . 2_575 ?
C1 Pt1 P1 102.07(9) . 2_575 ?
N1 Pt1 P1 101.13(9) . . ?
C1 Pt1 P1 173.85(8) . . ?
P1 Pt1 P1 77.25(3) 2_575 . ?
C20 P1 C14 105.37(14) . . ?
C20 P1 Pt1 113.40(10) . 2_575 ?
C14 P1 Pt1 109.84(10) . 2_575 ?
C20 P1 Pt1 116.22(10) . . ?
C14 P1 Pt1 109.24(10) . . ?
Pt1 P1 Pt1 102.75(3) 2_575 . ?
C13 N1 C10 118.0(3) . . ?
C13 N1 Pt1 129.0(2) . . ?
C10 N1 Pt1 113.0(2) . . ?
C2 C1 C6 117.0(3) . . ?
C2 C1 Pt1 130.1(2) . . ?
C6 C1 Pt1 112.6(2) . . ?
C1 C2 C3 121.9(3) . . ?
C1 C2 H2 119.1 . . ?
C3 C2 H2 119.1 . . ?
C4 C3 C2 120.4(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 119.6(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 118.2(3) . . ?
C4 C5 C7 124.0(3) . . ?
C6 C5 C7 117.8(3) . . ?
C1 C6 C5 122.7(3) . . ?
C1 C6 C10 117.1(3) . . ?
C5 C6 C10 120.1(3) . . ?
C8 C7 C5 121.9(3) . . ?
C8 C7 H7 119 . . ?
C5 C7 H7 119 . . ?
C7 C8 C9 121.2(3) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C11 C9 C10 117.8(3) . . ?
C11 C9 C8 123.9(3) . . ?
C10 C9 C8 118.3(3) . . ?
N1 C10 C9 122.3(3) . . ?
N1 C10 C6 117.0(3) . . ?
C9 C10 C6 120.6(3) . . ?
C12 C11 C9 119.7(3) . . ?
C12 C11 H11 120.2 . . ?
C9 C11 H11 120.2 . . ?
C11 C12 C13 120.4(4) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
N1 C13 C12 121.8(3) . . ?
N1 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C19 C14 C15 118.0(3) . . ?
C19 C14 P1 122.4(2) . . ?
C15 C14 P1 119.5(2) . . ?
C16 C15 C14 121.0(3) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C17 C16 C15 120.0(3) . . ?
C17 C16 H16 120 . . ?
C15 C16 H16 120 . . ?
C18 C17 C16 119.4(3) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 C19 120.7(3) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C18 C19 C14 120.9(3) . . ?
C18 C19 H19 119.6 . . ?
C14 C19 H19 119.6 . . ?
C21 C20 C25 118.4(3) . . ?
C21 C20 P1 125.3(2) . . ?
C25 C20 P1 116.3(2) . . ?
C22 C21 C20 121.0(3) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C23 C22 C21 119.7(3) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C23 C24 C25 120.5(3) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C24 C23 C22 119.7(3) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C24 C25 C20 120.6(3) . . ?
C24 C25 H25 119.7 . . ?
C20 C25 H25 119.7 . . ?
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
Pt1 N1 2.091(3) . ?
Pt1 C1 2.092(3) . ?
Pt1 P1 2.2982(8) 2_575 ?
Pt1 P1 2.3108(8) . ?
P1 C20 1.827(3) . ?
P1 C14 1.838(3) . ?
P1 Pt1 2.2982(8) 2_575 ?
N1 C13 1.353(5) . ?
N1 C10 1.383(4) . ?
C1 C2 1.366(5) . ?
C1 C6 1.393(4) . ?
C2 C3 1.400(5) . ?
C2 H2 0.93 . ?
C3 C4 1.381(5) . ?
C3 H3 0.93 . ?
C4 C5 1.391(5) . ?
C4 H4 0.93 . ?
C5 C6 1.410(4) . ?
C5 C7 1.444(5) . ?
C6 C10 1.426(5) . ?
C7 C8 1.345(6) . ?
C7 H7 0.93 . ?
C8 C9 1.433(5) . ?
C8 H8 0.93 . ?
C9 C11 1.401(5) . ?
C9 C10 1.410(4) . ?
C11 C12 1.371(5) . ?
C11 H11 0.93 . ?
C12 C13 1.399(5) . ?
C12 H12 0.93 . ?
C13 H13 0.93 . ?
C14 C19 1.391(5) . ?
C14 C15 1.396(4) . ?
C15 C16 1.393(5) . ?
C15 H15 0.93 . ?
C16 C17 1.382(6) . ?
C16 H16 0.93 . ?
C17 C18 1.380(6) . ?
C17 H17 0.93 . ?
C18 C19 1.384(5) . ?
C18 H18 0.93 . ?
C19 H19 0.93 . ?
C20 C21 1.392(4) . ?
C20 C25 1.397(4) . ?
C21 C22 1.391(5) . ?
C21 H21 0.93 . ?
C22 C23 1.391(5) . ?
C22 H22 0.93 . ?
C24 C23 1.381(5) . ?
C24 C25 1.384(5) . ?
C24 H24 0.93 . ?
C23 H23 0.93 . ?
C25 H25 0.93 . ?
