#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:20:53 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178895 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/24/4112443.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_4112443
loop_
_publ_author_name
'Wei Lu'
'Bao-Xiu Mi'
'Michael C. W. Chan'
'Zheng Hui'
'Chi-Ming Che'
'Nianyong Zhu'
'Shuit-Tong Lee'
_publ_contact_author_address
;
Department of Chemistry, The University of Hong Kong, 
Pokfulam Road, Hong kong SAR, China
;
_publ_contact_author_name        'Chi-Ming Che (Prof.)'
_publ_section_title
;
 Light-Emitting Tridentate Cyclometalated Platinum(II) Complexes
 Containing σ-Alkynyl Auxiliaries: Tuning of Photo- and
 Electrophosphorescence
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4958
_journal_page_last               4971
_journal_paper_doi               10.1021/ja0317776
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C25 H20 N2 Pt1 Si1'
_chemical_formula_sum            'C23 H20 N2 Pt Si'
_chemical_formula_weight         547.59
_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                 98.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.684(3)
_cell_length_b                   11.146(2)
_cell_length_c                   12.828(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2075.2(8)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.892
_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  0.0702
_diffrn_reflns_av_sigmaI/netI    0.0824
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8345
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    6.829
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.834
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0384
_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)+(0.0365P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                2436
_reflns_number_total             3453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0317776si20031217_101956_4.cif
_cod_data_source_block           mar204a
_cod_original_cell_volume        2075.2(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4112443
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
Pt1 Pt 0.085634(19) 0.05531(2) 0.33743(2) 0.06212(14) Uani 1 1 d .
Si1 Si 0.46543(14) -0.2351(2) 0.0888(2) 0.0809(7) Uani 1 1 d .
N1 N 0.1622(5) 0.1170(6) 0.4756(6) 0.0832(19) Uani 1 1 d .
N2 N -0.0132(4) 0.1245(5) 0.4106(5) 0.0629(15) Uani 1 1 d .
C1 C 0.2562(6) 0.1133(8) 0.5056(8) 0.089(3) Uani 1 1 d .
H1 H 0.2927 0.0778 0.4609 0.106 Uiso 1 1 calc R
C2 C 0.2974(6) 0.1607(9) 0.5996(9) 0.106(3) Uani 1 1 d .
H2 H 0.3611 0.1580 0.6181 0.127 Uiso 1 1 calc R
C3 C 0.2431(8) 0.2130(10) 0.6672(8) 0.108(3) Uani 1 1 d .
H3 H 0.2704 0.2464 0.7308 0.130 Uiso 1 1 calc R
C4 C 0.1507(7) 0.2149(8) 0.6402(7) 0.089(3) Uani 1 1 d .
H4 H 0.1148 0.2485 0.6863 0.107 Uiso 1 1 calc R
C5 C 0.1082(6) 0.1678(7) 0.5449(7) 0.076(2) Uani 1 1 d .
C6 C 0.0095(6) 0.1716(6) 0.5076(6) 0.070(2) Uani 1 1 d .
C7 C -0.0576(7) 0.2176(7) 0.5589(7) 0.090(3) Uani 1 1 d .
H7 H -0.0432 0.2507 0.6260 0.108 Uiso 1 1 calc R
C8 C -0.1476(7) 0.2135(8) 0.5080(9) 0.094(3) Uani 1 1 d .
H8 H -0.1944 0.2434 0.5421 0.113 Uiso 1 1 calc R
C9 C -0.1695(6) 0.1670(7) 0.4095(8) 0.087(3) Uani 1 1 d .
H9 H -0.2302 0.1666 0.3760 0.105 Uiso 1 1 calc R
C10 C -0.1001(5) 0.1204(6) 0.3598(6) 0.067(2) Uani 1 1 d .
C11 C -0.1069(6) 0.0621(6) 0.2568(7) 0.073(2) Uani 1 1 d .
C12 C -0.1915(6) 0.0488(7) 0.1902(9) 0.088(3) Uani 1 1 d .
H12 H -0.2458 0.0766 0.2108 0.106 Uiso 1 1 calc R
C13 C -0.1926(8) -0.0072(10) 0.0920(10) 0.108(3) Uani 1 1 d .
H13 H -0.2478 -0.0158 0.0464 0.130 Uiso 1 1 calc R
C14 C -0.1123(8) -0.0491(7) 0.0634(9) 0.102(3) Uani 1 1 d .
H14 H -0.1127 -0.0855 -0.0019 0.123 Uiso 1 1 calc R
C15 C -0.0293(7) -0.0368(7) 0.1332(8) 0.089(3) Uani 1 1 d .
H15 H 0.0247 -0.0673 0.1139 0.107 Uiso 1 1 calc R
C16 C -0.0257(6) 0.0186(6) 0.2281(6) 0.066(2) Uani 1 1 d .
C17 C 0.1839(5) -0.0127(7) 0.2679(6) 0.0651(19) Uani 1 1 d .
C18 C 0.2456(6) -0.0546(6) 0.2280(6) 0.071(2) Uani 1 1 d .
C19 C 0.3156(5) -0.1052(7) 0.1830(6) 0.0678(19) Uani 1 1 d .
C20 C 0.3758(5) -0.1542(7) 0.1444(6) 0.077(2) Uani 1 1 d .
C21 C 0.4972(8) -0.3690(10) 0.1721(11) 0.167(5) Uani 1 1 d .
H21A H 0.5440 -0.4136 0.1442 0.251 Uiso 1 1 calc R
H21B H 0.4438 -0.4187 0.1724 0.251 Uiso 1 1 calc R
H21C H 0.5202 -0.3441 0.2429 0.251 Uiso 1 1 calc R
C22 C 0.5690(5) -0.1372(9) 0.0887(8) 0.109(3) Uani 1 1 d .
H22A H 0.6154 -0.1806 0.0591 0.163 Uiso 1 1 calc R
H22B H 0.5927 -0.1142 0.1598 0.163 Uiso 1 1 calc R
H22C H 0.5519 -0.0668 0.0473 0.163 Uiso 1 1 calc R
C23 C 0.4190(6) -0.2808(13) -0.0468(8) 0.171(6) Uani 1 1 d .
H23A H 0.4654 -0.3238 -0.0768 0.256 Uiso 1 1 calc R
H23B H 0.4010 -0.2109 -0.0885 0.256 Uiso 1 1 calc R
H23C H 0.3664 -0.3317 -0.0457 0.256 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
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C17 Pt1 N2 179.1(3)
C17 Pt1 C16 100.3(3)
N2 Pt1 C16 80.5(3)
C17 Pt1 N1 100.2(3)
N2 Pt1 N1 78.9(3)
C16 Pt1 N1 159.5(3)
C20 Si1 C23 108.7(4)
C20 Si1 C21 107.8(5)
C23 Si1 C21 110.3(7)
C20 Si1 C22 110.3(4)
C23 Si1 C22 110.2(5)
C21 Si1 C22 109.7(5)
C1 N1 C5 118.4(8)
C1 N1 Pt1 128.4(7)
C5 N1 Pt1 113.2(6)
C10 N2 C6 123.1(6)
C10 N2 Pt1 117.7(5)
C6 N2 Pt1 119.3(5)
C2 C1 N1 121.7(9)
C1 C2 C3 119.4(9)
C4 C3 C2 119.7(10)
C3 C4 C5 121.4(9)
C4 C5 N1 119.4(8)
C4 C5 C6 124.8(8)
N1 C5 C6 115.7(7)
N2 C6 C7 119.9(8)
N2 C6 C5 112.8(7)
C7 C6 C5 127.3(9)
C6 C7 C8 117.8(9)
C9 C8 C7 121.7(8)
C8 C9 C10 119.1(8)
N2 C10 C9 118.4(8)
N2 C10 C11 112.4(7)
C9 C10 C11 129.1(8)
C16 C11 C12 121.2(9)
C16 C11 C10 116.9(8)
C12 C11 C10 121.9(8)
C13 C12 C11 118.7(10)
C14 C13 C12 119.9(10)
C13 C14 C15 119.6(10)
C16 C15 C14 121.8(10)
C15 C16 C11 118.6(9)
C15 C16 Pt1 129.0(7)
C11 C16 Pt1 112.4(6)
C18 C17 Pt1 178.2(7)
C17 C18 C19 178.6(9)
C20 C19 C18 177.4(9)
C19 C20 Si1 177.2(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pt1 C17 1.960(8)
Pt1 N2 1.999(5)
Pt1 C16 2.027(9)
Pt1 N1 2.066(7)
Si1 C20 1.827(8)
Si1 C23 1.841(9)
Si1 C21 1.854(11)
Si1 C22 1.871(9)
N1 C1 1.377(10)
N1 C5 1.398(10)
N2 C10 1.342(9)
N2 C6 1.345(9)
C1 C2 1.371(12)
C2 C3 1.393(13)
C3 C4 1.347(12)
C4 C5 1.388(11)
C5 C6 1.457(10)
C6 C7 1.365(10)
C7 C8 1.383(12)
C8 C9 1.358(12)
C9 C10 1.382(10)
C10 C11 1.463(11)
C11 C16 1.387(11)
C11 C12 1.405(12)
C12 C13 1.404(14)
C13 C14 1.370(14)
C14 C15 1.405(14)
C15 C16 1.359(11)
C17 C18 1.201(10)
C18 C19 1.373(11)
C19 C20 1.208(10)
