#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:09:12 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178837 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/91/4109194.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_4109194
loop_
_publ_author_name
'Shu-Bin Zhao'
'Rui-Yao Wang'
'Suning Wang'
_publ_section_title
;
 Intramolecular C-H Activation Directed Self-Assembly of an
 Organoplatinum(II) Molecular Square
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3092
_journal_page_last               3093
_journal_paper_doi               10.1021/ja0702770
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C24 H19 N3 Pt'
_chemical_formula_weight         544.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.6256(17)
_cell_length_b                   17.061(2)
_cell_length_c                   17.386(2)
_cell_measurement_reflns_used    5664
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.32
_cell_volume                     3745.0(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      180(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32073
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    7.508
_exptl_absorpt_correction_T_max  0.8643
_exptl_absorpt_correction_T_min  0.6615
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.467
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0309
_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)+(0.0712P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                2801
_reflns_number_total             3300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0702770si20070119_041333.cif
_cod_data_source_block           sbptph
_cod_original_cell_volume        3745.0(9)
_cod_database_code               4109194
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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
Pt1 Pt 0.722080(14) 0.881625(11) 0.607443(10) 0.02086(11) Uani 1 1 d .
N1 N 0.6146(3) 0.8052(2) 0.5528(2) 0.0229(8) Uani 1 1 d .
N2 N 0.5475(3) 0.9073(2) 0.4684(2) 0.0270(9) Uani 1 1 d .
N3 N 0.7176(3) 0.9528(2) 0.5059(2) 0.0262(10) Uani 1 1 d .
C1 C 0.5987(4) 0.7303(3) 0.5747(3) 0.0281(11) Uani 1 1 d .
H1A H 0.6477 0.7076 0.6097 0.034 Uiso 1 1 calc R
C2 C 0.5152(5) 0.6845(3) 0.5494(3) 0.0343(13) Uani 1 1 d .
H2A H 0.5090 0.6315 0.5658 0.041 Uiso 1 1 calc R
C3 C 0.4407(4) 0.7161(3) 0.4999(3) 0.0356(13) Uani 1 1 d .
H3A H 0.3820 0.6861 0.4826 0.043 Uiso 1 1 calc R
C4 C 0.4546(4) 0.7930(3) 0.4767(3) 0.0281(11) Uani 1 1 d .
C5 C 0.3979(5) 0.8475(3) 0.4278(3) 0.0431(14) Uani 1 1 d .
H5A H 0.3321 0.8378 0.4032 0.052 Uiso 1 1 calc R
C6 C 0.4550(5) 0.9152(3) 0.4233(3) 0.0360(13) Uani 1 1 d .
H6A H 0.4358 0.9603 0.3945 0.043 Uiso 1 1 calc R
C7 C 0.5443(4) 0.8330(3) 0.5020(3) 0.0255(11) Uani 1 1 d .
C8 C 0.6346(4) 0.9571(3) 0.4578(3) 0.0279(11) Uani 1 1 d .
C9 C 0.6319(5) 1.0112(3) 0.3961(3) 0.0389(15) Uani 1 1 d .
H9A H 0.5726 1.0131 0.3626 0.047 Uiso 1 1 calc R
C10 C 0.7156(5) 1.0607(4) 0.3854(3) 0.0436(18) Uani 1 1 d .
H10A H 0.7149 1.0981 0.3450 0.052 Uiso 1 1 calc R
C11 C 0.8020(5) 1.0554(3) 0.4349(3) 0.0413(14) Uani 1 1 d .
H11A H 0.8611 1.0893 0.4290 0.050 Uiso 1 1 calc R
C12 C 0.8004(4) 1.0007(3) 0.4919(3) 0.0343(13) Uani 1 1 d .
H12A H 0.8612 0.9960 0.5238 0.041 Uiso 1 1 calc R
C13 C 0.7254(4) 0.8195(3) 0.7054(3) 0.0231(11) Uani 1 1 d .
C14 C 0.6348(4) 0.8112(3) 0.7501(3) 0.0291(11) Uani 1 1 d .
H14A H 0.5701 0.8330 0.7324 0.035 Uiso 1 1 calc R
C15 C 0.6364(4) 0.7714(3) 0.8209(3) 0.0303(12) Uani 1 1 d .
H15A H 0.5730 0.7668 0.8500 0.036 Uiso 1 1 calc R
C16 C 0.7281(5) 0.7393(3) 0.8484(3) 0.0346(14) Uani 1 1 d .
H16A H 0.7292 0.7134 0.8967 0.041 Uiso 1 1 calc R
C17 C 0.8200(5) 0.7451(3) 0.8041(3) 0.0353(13) Uani 1 1 d .
H17A H 0.8841 0.7226 0.8222 0.042 Uiso 1 1 calc R
C18 C 0.8181(4) 0.7838(3) 0.7338(3) 0.0283(11) Uani 1 1 d .
H18A H 0.8811 0.7862 0.7040 0.034 Uiso 1 1 calc R
C19 C 0.8186(4) 0.9582(3) 0.6606(3) 0.0250(10) Uani 1 1 d .
C20 C 0.9270(4) 0.9473(3) 0.6650(3) 0.0317(12) Uani 1 1 d .
H20A H 0.9566 0.9000 0.6459 0.038 Uiso 1 1 calc R
C21 C 0.9952(5) 1.0044(3) 0.6970(3) 0.0381(13) Uani 1 1 d .
H21A H 1.0692 0.9951 0.6998 0.046 Uiso 1 1 calc R
C22 C 0.9535(5) 1.0729(3) 0.7237(3) 0.0405(14) Uani 1 1 d .
H22A H 0.9988 1.1124 0.7437 0.049 Uiso 1 1 calc R
C23 C 0.8454(5) 1.0847(3) 0.7216(3) 0.0386(14) Uani 1 1 d .
H23A H 0.8161 1.1318 0.7417 0.046 Uiso 1 1 calc R
C24 C 0.7799(4) 1.0283(3) 0.6905(3) 0.0278(12) Uani 1 1 d .
H24A H 0.7058 1.0375 0.6894 0.033 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
C13 Pt1 C19 86.60(18)
C13 Pt1 N1 93.98(17)
C19 Pt1 N1 177.16(18)
C13 Pt1 N3 177.36(17)
C19 Pt1 N3 91.51(16)
N1 Pt1 N3 87.82(15)
C7 N1 C1 115.0(4)
C7 N1 Pt1 120.3(3)
C1 N1 Pt1 123.7(3)
C7 N2 C8 128.9(4)
C7 N2 C6 107.2(4)
C8 N2 C6 121.2(4)
C8 N3 C12 117.3(4)
C8 N3 Pt1 124.4(3)
C12 N3 Pt1 118.1(3)
N1 C1 C2 124.0(5)
C3 C2 C1 119.7(5)
C4 C3 C2 117.7(5)
C3 C4 C7 118.4(5)
C3 C4 C5 135.9(5)
C7 C4 C5 105.7(4)
C6 C5 C4 108.5(5)
C5 C6 N2 108.9(5)
N1 C7 C4 125.0(4)
N1 C7 N2 125.4(4)
C4 C7 N2 109.6(4)
N3 C8 N2 119.8(4)
N3 C8 C9 121.8(5)
N2 C8 C9 118.4(5)
C10 C9 C8 119.2(5)
C9 C10 C11 118.8(5)
C12 C11 C10 118.9(6)
N3 C12 C11 123.9(5)
C14 C13 C18 116.4(5)
C14 C13 Pt1 120.7(4)
C18 C13 Pt1 122.9(4)
C13 C14 C15 121.8(5)
C16 C15 C14 120.7(5)
C15 C16 C17 118.9(5)
C18 C17 C16 120.3(5)
C17 C18 C13 121.8(5)
C20 C19 C24 116.2(4)
C20 C19 Pt1 122.5(4)
C24 C19 Pt1 121.1(4)
C19 C20 C21 122.1(5)
C22 C21 C20 119.3(6)
C21 C22 C23 119.8(5)
C22 C23 C24 120.0(5)
C23 C24 C19 122.4(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pt1 C13 2.007(5)
Pt1 C19 2.012(5)
Pt1 N1 2.107(4)
Pt1 N3 2.143(4)
N1 C7 1.339(6)
N1 C1 1.350(6)
N2 C7 1.396(6)
N2 C8 1.403(6)
N2 C6 1.412(7)
N3 C8 1.343(6)
N3 C12 1.350(7)
C1 C2 1.385(7)
C2 C3 1.384(8)
C3 C4 1.383(7)
C4 C7 1.394(7)
C4 C5 1.449(7)
C5 C6 1.363(8)
C8 C9 1.415(7)
C9 C10 1.365(9)
C10 C11 1.393(8)
C11 C12 1.361(8)
C13 C14 1.390(7)
C13 C18 1.409(7)
C14 C15 1.405(7)
C15 C16 1.367(8)
C16 C17 1.395(8)
C17 C18 1.390(7)
C19 C20 1.383(7)
C19 C24 1.392(7)
C20 C21 1.413(7)
C21 C22 1.364(8)
C22 C23 1.380(8)
C23 C24 1.380(7)
