#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/10/4001021.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_4001021
loop_
_publ_author_name
'Drew, Steven M.'
'Smith, Lisa I.'
'McGee, Kari A.'
'Mann, Kent R.'
_publ_section_title
;
 A Platinum(II) Extended Linear Chain Material That Selectively Uptakes
 Benzene
;
_journal_issue                   14
_journal_name_full               'Chemistry of Materials'
_journal_page_first              3117
_journal_paper_doi               10.1021/cm900401u
_journal_volume                  21
_journal_year                    2009
_chemical_formula_moiety         'C10 H14 N4 Pt, 0.5(C6 H6)'
_chemical_formula_sum            'C13 H17 N4 Pt'
_chemical_formula_weight         424.40
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.746(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.544(2)
_cell_length_b                   6.8773(11)
_cell_length_c                   18.322(3)
_cell_measurement_reflns_used    2833
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.27
_cell_volume                     1547.5(4)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14607
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.81
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    9.057
_exptl_absorpt_correction_T_max  .257
_exptl_absorpt_correction_T_min  .153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             804
_exptl_crystal_recrystallization_method 'Acetonitrile, Benzene'
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .15
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0197
_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)+(0.0226P)²+1.0901P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0426
_refine_ls_wR_factor_ref         0.0445
_reflns_number_gt                2426
_reflns_number_total             2736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm900401u_si_002.cif
_cod_data_source_block           07292
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4001021
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 0.271292(12) 0.28116(2) 0.759007(8) 0.02293(6) Uani 1 1 d .
N1 N 0.5248(3) 0.2873(5) 0.7733(2) 0.0417(10) Uani 1 1 d .
N2 N 0.3047(3) 0.2758(5) 0.9337(2) 0.0373(9) Uani 1 1 d .
N3 N 0.0187(3) 0.2701(5) 0.7425(2) 0.0340(8) Uani 1 1 d .
N4 N 0.2310(3) 0.2929(4) 0.5853(2) 0.0298(8) Uani 1 1 d .
C1 C 0.4322(4) 0.2854(5) 0.7691(2) 0.0287(9) Uani 1 1 d .
C2 C 0.2927(3) 0.2788(5) 0.8693(3) 0.0299(9) Uani 1 1 d .
C3 C 0.1118(4) 0.2764(5) 0.7502(2) 0.0266(9) Uani 1 1 d .
C4 C 0.2495(3) 0.2863(5) 0.6487(3) 0.0287(9) Uani 1 1 d .
C5 C -0.0986(4) 0.2492(7) 0.7296(3) 0.0455(12) Uani 1 1 d .
H5A H -0.1157 0.1086 0.7352 0.055 Uiso 1 1 calc R
C6 C -0.1431(4) 0.3614(9) 0.7862(3) 0.0629(15) Uani 1 1 d .
H6A H -0.1103 0.3141 0.8362 0.094 Uiso 1 1 calc R
H6B H -0.2223 0.3442 0.7774 0.094 Uiso 1 1 calc R
H6C H -0.1261 0.4996 0.7823 0.094 Uiso 1 1 calc R
C7 C -0.1453(5) 0.3080(9) 0.6506(3) 0.0695(17) Uani 1 1 d .
H7A H -0.1128 0.2286 0.6165 0.104 Uiso 1 1 calc R
H7B H -0.1293 0.4455 0.6438 0.104 Uiso 1 1 calc R
H7C H -0.2244 0.2883 0.6401 0.104 Uiso 1 1 calc R
C8 C 0.1931(3) 0.3088(6) 0.5052(2) 0.0347(10) Uani 1 1 d .
H8A H 0.1998 0.4474 0.4903 0.042 Uiso 1 1 calc R
C9 C 0.2615(4) 0.1840(7) 0.4647(3) 0.0480(12) Uani 1 1 d .
H9A H 0.3378 0.2251 0.4784 0.072 Uiso 1 1 calc R
H9B H 0.2358 0.1985 0.4108 0.072 Uiso 1 1 calc R
H9C H 0.2554 0.0476 0.4787 0.072 Uiso 1 1 calc R
C10 C 0.0756(4) 0.2527(7) 0.4871(3) 0.0541(14) Uani 1 1 d .
H10A H 0.0343 0.3378 0.5140 0.081 Uiso 1 1 calc R
H10B H 0.0678 0.1174 0.5020 0.081 Uiso 1 1 calc R
H10C H 0.0477 0.2661 0.4333 0.081 Uiso 1 1 calc R
C11 C 0.4735(5) 0.5914(10) 0.4326(3) 0.0675(16) Uani 1 1 d .
H11A H 0.4551 0.6556 0.3858 0.081 Uiso 1 1 calc R
C12 C 0.5439(4) 0.4396(9) 0.4418(3) 0.0629(17) Uani 1 1 d .
H12A H 0.5745 0.3968 0.4012 0.076 Uiso 1 1 calc R
C13 C 0.5708(4) 0.3481(8) 0.5090(4) 0.0684(17) Uani 1 1 d .
H13A H 0.6204 0.2422 0.5153 0.082 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'
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_1
_geom_angle_site_symmetry_3
C3 Pt1 C4 89.39(17) . .
C3 Pt1 C2 90.47(17) . .
C4 Pt1 C2 179.44(16) . .
C3 Pt1 C1 179.37(16) . .
C4 Pt1 C1 91.23(17) . .
C2 Pt1 C1 88.92(17) . .
C3 N3 C5 175.7(4) . .
C4 N4 C8 172.4(4) . .
N1 C1 Pt1 178.6(4) . .
N2 C2 Pt1 179.4(4) . .
N3 C3 Pt1 177.5(4) . .
N4 C4 Pt1 176.1(4) . .
N3 C5 C6 110.2(4) . .
N3 C5 C7 108.4(4) . .
C6 C5 C7 113.8(4) . .
N3 C5 H5A 108.1 . .
C6 C5 H5A 108.1 . .
C7 C5 H5A 108.1 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N4 C8 C10 108.1(4) . .
N4 C8 C9 110.6(4) . .
C10 C8 C9 112.2(4) . .
N4 C8 H8A 108.6 . .
C10 C8 H8A 108.6 . .
C9 C8 H8A 108.6 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C12 C11 C13 119.7(5) . 3_666
C12 C11 H11A 120.1 . .
C13 C11 H11A 120.1 3_666 .
C11 C12 C13 120.2(5) . .
C11 C12 H12A 119.9 . .
C13 C12 H12A 119.9 . .
C12 C13 C11 120.1(5) . 3_666
C12 C13 H13A 119.9 . .
C11 C13 H13A 119.9 3_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 C3 1.975(4) .
Pt1 C4 1.983(5) .
Pt1 C2 1.984(5) .
Pt1 C1 1.990(5) .
N1 C1 1.148(6) .
N2 C2 1.158(6) .
N3 C3 1.148(6) .
N3 C5 1.449(6) .
N4 C4 1.139(5) .
N4 C8 1.452(5) .
C5 C6 1.490(7) .
C5 C7 1.502(8) .
C5 H5A 1.0000 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C10 1.494(7) .
C8 C9 1.510(6) .
C8 H8A 1.0000 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.356(8) .
C11 C13 1.367(8) 3_666
C11 H11A 0.9500 .
C12 C13 1.363(8) .
C12 H12A 0.9500 .
C13 C11 1.367(8) 3_666
C13 H13A 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C13 C11 C12 C13 -0.4(9) 3_666 .
C11 C12 C13 C11 0.4(9) . 3_666
