#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/13/7011336.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_7011336
loop_
_publ_author_name
'Muhammad S. Khan'
'Muna R. A. Al-Mandhary'
'Mohammed K. Al-Suti'
'Abdul Khader Hisahm'
'Paul R. Raithby'
'Birte Ahrens'
'Mary F. Mahon'
'Louise Male'
'Elisabeth A. Marseglia'
'Emilio Tedesco'
'Richard H. Friend'
'Anna Köhler'
'Neil Feeder'
'Simon J. Teat'
_publ_section_title
;
 Structural characterisation of a series of acetylide-functionalised
 oligopyridines and the synthesis, characterisation and optical
 spectroscopy of platinum di-ynes and poly-ynes containing oligopyridyl
 linker groups in the backbone
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1358
_journal_page_last               1368
_journal_paper_doi               10.1039/b110658a
_journal_year                    2002
_chemical_formula_sum            'C25 H27 N3 Si2'
_chemical_formula_weight         425.68
_chemical_name_systematic
; 
Compound 3a
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.891(8)
_cell_angle_beta                 86.268(10)
_cell_angle_gamma                82.049(10)
_cell_formula_units_Z            2
_cell_length_a                   6.3543(8)
_cell_length_b                   10.844(2)
_cell_length_c                   17.722(4)
_cell_measurement_reflns_used    11843
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     1202.9(4)
_computing_cell_refinement       'Nonius HKL Scalepack'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius HKL Denzo & Scalepack'
_computing_molecular_graphics    'XSEED (J. Barbour, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'omega and phi 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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.1355
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7566
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.11
_diffrn_standards_number         'not applicable'
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.9886
_exptl_absorpt_correction_T_min  0.9557
_exptl_absorpt_correction_type   SORTAV
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    'methyls rigid, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5373
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.1393
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0444P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                2787
_reflns_number_total             5373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110658a.txt
_cod_data_source_block           pr9942
_cod_original_cell_volume        1202.8(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011336
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
Si1 Si 0.55690(10) 0.25829(7) 0.16878(4) 0.0327(2) Uani 1 1 d . . .
Si2 Si 0.14411(11) 1.25859(7) 0.87778(4) 0.0356(2) Uani 1 1 d . . .
C1 C 0.4625(4) 0.1048(3) 0.18148(18) 0.0535(8) Uani 1 1 d . . .
H1A H 0.5121 0.0607 0.2291 0.080 Uiso 1 1 calc R . .
H1B H 0.5183 0.0558 0.1390 0.080 Uiso 1 1 calc R . .
H1C H 0.3066 0.1160 0.1832 0.080 Uiso 1 1 calc R . .
C2 C 0.5013(4) 0.3361(3) 0.07315(15) 0.0527(8) Uani 1 1 d . . .
H2A H 0.3475 0.3480 0.0668 0.079 Uiso 1 1 calc R . .
H2B H 0.5733 0.2839 0.0343 0.079 Uiso 1 1 calc R . .
H2C H 0.5536 0.4175 0.0679 0.079 Uiso 1 1 calc R . .
C3 C 0.8473(4) 0.2386(3) 0.18094(16) 0.0489(8) Uani 1 1 d . . .
H3A H 0.9004 0.3192 0.1694 0.073 Uiso 1 1 calc R . .
H3B H 0.9194 0.1784 0.1464 0.073 Uiso 1 1 calc R . .
H3C H 0.8758 0.2076 0.2334 0.073 Uiso 1 1 calc R . .
C4 C 0.4062(4) 0.3577(2) 0.23822(14) 0.0335(6) Uani 1 1 d . . .
C5 C 0.2847(4) 0.4201(2) 0.27927(14) 0.0314(6) Uani 1 1 d . . .
N1 N 0.1991(3) 0.55682(18) 0.37944(11) 0.0273(5) Uani 1 1 d D . .
C6 C 0.1277(3) 0.4943(2) 0.32622(13) 0.0265(6) Uani 1 1 d D . .
C7 C -0.0880(3) 0.4984(2) 0.31399(14) 0.0305(6) Uani 1 1 d D . .
H7 H -0.1330 0.4507 0.2770 0.037 Uiso 1 1 calc R . .
C8 C -0.2340(3) 0.5727(2) 0.35651(13) 0.0292(6) Uani 1 1 d D . .
H8 H -0.3819 0.5773 0.3494 0.035 Uiso 1 1 calc R . .
C9 C -0.1628(3) 0.6403(2) 0.40949(13) 0.0269(6) Uani 1 1 d D . .
H9 H -0.2608 0.6946 0.4381 0.032 Uiso 1 1 calc R . .
C10 C 0.0538(3) 0.6283(2) 0.42069(13) 0.0238(6) Uani 1 1 d D . .
N2 N 0.0019(3) 0.78126(18) 0.51440(11) 0.0256(5) Uani 1 1 d D . .
C11 C 0.1364(3) 0.6925(2) 0.48159(13) 0.0249(6) Uani 1 1 d D . .
C12 C 0.3437(3) 0.6567(2) 0.50383(13) 0.0260(6) Uani 1 1 d D . .
H12 H 0.4348 0.5934 0.4795 0.031 Uiso 1 1 calc R . .
C13 C 0.4146(3) 0.7146(2) 0.56165(13) 0.0302(6) Uani 1 1 d D . .
H13 H 0.5553 0.6916 0.5779 0.036 Uiso 1 1 calc R . .
C14 C 0.2788(3) 0.8062(2) 0.59556(13) 0.0280(6) Uani 1 1 d D . .
H14 H 0.3235 0.8468 0.6359 0.034 Uiso 1 1 calc R . .
C15 C 0.0747(3) 0.8384(2) 0.56969(13) 0.0247(6) Uani 1 1 d D . .
N3 N 0.0041(3) 0.99868(19) 0.65675(11) 0.0282(5) Uani 1 1 d D . .
C16 C -0.0743(3) 0.9403(2) 0.60299(13) 0.0251(6) Uani 1 1 d D . .
C17 C -0.2813(3) 0.9727(2) 0.57986(13) 0.0285(6) Uani 1 1 d D . .
H17 H -0.3317 0.9305 0.5413 0.034 Uiso 1 1 calc R . .
C18 C -0.4123(3) 1.0670(2) 0.61369(14) 0.0311(6) Uani 1 1 d D . .
H18 H -0.5550 1.0895 0.5995 0.037 Uiso 1 1 calc R . .
C19 C -0.3330(4) 1.1282(2) 0.66848(14) 0.0310(6) Uani 1 1 d D . .
H19 H -0.4189 1.1946 0.6918 0.037 Uiso 1 1 calc R . .
C20 C -0.1242(3) 1.0903(2) 0.68879(13) 0.0279(6) Uani 1 1 d D . .
C21 C -0.0359(4) 1.1497(2) 0.74756(14) 0.0315(6) Uani 1 1 d . . .
C22 C 0.0359(4) 1.1953(2) 0.79775(15) 0.0363(7) Uani 1 1 d . . .
C23 C 0.4184(4) 1.2904(3) 0.85144(15) 0.0494(8) Uani 1 1 d . . .
H23A H 0.5086 1.2121 0.8415 0.074 Uiso 1 1 calc R . .
H23B H 0.4738 1.3278 0.8931 0.074 Uiso 1 1 calc R . .
H23C H 0.4183 1.3483 0.8057 0.074 Uiso 1 1 calc R . .
C24 C -0.0270(4) 1.4043(3) 0.90117(16) 0.0463(8) Uani 1 1 d . . .
H24A H -0.0411 1.4623 0.8555 0.069 Uiso 1 1 calc R . .
H24B H 0.0376 1.4430 0.9403 0.069 Uiso 1 1 calc R . .
H24C H -0.1679 1.3848 0.9201 0.069 Uiso 1 1 calc R . .
C25 C 0.1387(5) 1.1395(3) 0.96011(16) 0.0602(9) Uani 1 1 d . . .
H25A H -0.0066 1.1194 0.9704 0.090 Uiso 1 1 calc R . .
H25B H 0.1860 1.1727 1.0048 0.090 Uiso 1 1 calc R . .
H25C H 0.2338 1.0637 0.9484 0.090 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'
Si Si 0.0817 0.0704 '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
C1 Si1 C4 107.80(12) . . ?
C1 Si1 C3 109.35(13) . . ?
C4 Si1 C3 112.35(12) . . ?
C1 Si1 C2 111.19(14) . . ?
C4 Si1 C2 106.92(12) . . ?
C3 Si1 C2 109.22(13) . . ?
C22 Si2 C23 109.37(11) . . ?
C22 Si2 C24 109.09(12) . . ?
C23 Si2 C24 110.29(13) . . ?
C22 Si2 C25 107.35(13) . . ?
C23 Si2 C25 111.06(14) . . ?
C24 Si2 C25 109.62(13) . . ?
C5 C4 Si1 171.6(2) . . ?
C4 C5 C6 176.6(2) . . ?
C10 N1 C6 117.43(18) . . ?
N1 C6 C7 123.0(2) . . ?
N1 C6 C5 117.82(19) . . ?
C7 C6 C5 119.2(2) . . ?
C8 C7 C6 118.6(2) . . ?
C7 C8 C9 119.0(2) . . ?
C8 C9 C10 119.4(2) . . ?
N1 C10 C9 122.5(2) . . ?
N1 C10 C11 116.38(19) . . ?
C9 C10 C11 121.1(2) . . ?
C11 N2 C15 117.72(19) . . ?
N2 C11 C12 122.6(2) . . ?
N2 C11 C10 117.47(19) . . ?
C12 C11 C10 119.9(2) . . ?
C13 C12 C11 119.0(2) . . ?
C14 C13 C12 119.1(2) . . ?
C13 C14 C15 118.8(2) . . ?
N2 C15 C14 122.8(2) . . ?
N2 C15 C16 116.76(19) . . ?
C14 C15 C16 120.4(2) . . ?
C20 N3 C16 118.0(2) . . ?
N3 C16 C17 122.3(2) . . ?
N3 C16 C15 115.7(2) . . ?
C17 C16 C15 121.9(2) . . ?
C18 C17 C16 119.1(2) . . ?
C17 C18 C19 119.1(2) . . ?
C18 C19 C20 118.5(2) . . ?
N3 C20 C19 123.0(2) . . ?
N3 C20 C21 116.5(2) . . ?
C19 C20 C21 120.5(2) . . ?
C22 C21 C20 177.8(3) . . ?
C21 C22 Si2 177.2(3) . . ?
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
Si1 C1 1.837(3) . ?
Si1 C4 1.841(3) . ?
Si1 C3 1.852(2) . ?
Si1 C2 1.857(3) . ?
Si2 C22 1.840(3) . ?
Si2 C23 1.846(2) . ?
Si2 C24 1.853(3) . ?
Si2 C25 1.862(3) . ?
C4 C5 1.206(3) . ?
C5 C6 1.457(3) . ?
N1 C10 1.343(3) . ?
N1 C6 1.345(3) . ?
C6 C7 1.396(3) . ?
C7 C8 1.374(3) . ?
C8 C9 1.376(3) . ?
C9 C10 1.390(3) . ?
C10 C11 1.494(3) . ?
N2 C11 1.343(3) . ?
N2 C15 1.343(3) . ?
C11 C12 1.393(3) . ?
C12 C13 1.379(3) . ?
C13 C14 1.376(3) . ?
C14 C15 1.392(3) . ?
C15 C16 1.489(3) . ?
N3 C20 1.338(3) . ?
N3 C16 1.347(3) . ?
C16 C17 1.393(3) . ?
C17 C18 1.381(3) . ?
C18 C19 1.381(3) . ?
C19 C20 1.394(3) . ?
C20 C21 1.453(3) . ?
C21 C22 1.199(3) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 Si1 C4 C5 -59.2(17) . . . . ?
C3 Si1 C4 C5 -180(100) . . . . ?
C2 Si1 C4 C5 60.4(17) . . . . ?
Si1 C4 C5 C6 -4(6) . . . . ?
C10 N1 C6 C7 -1.7(4) . . . . ?
C10 N1 C6 C5 177.8(2) . . . . ?
C4 C5 C6 N1 -173(5) . . . . ?
C4 C5 C6 C7 6(5) . . . . ?
N1 C6 C7 C8 2.1(4) . . . . ?
C5 C6 C7 C8 -177.4(2) . . . . ?
C6 C7 C8 C9 0.0(4) . . . . ?
C7 C8 C9 C10 -2.3(4) . . . . ?
C6 N1 C10 C9 -0.8(3) . . . . ?
C6 N1 C10 C11 177.5(2) . . . . ?
C8 C9 C10 N1 2.8(4) . . . . ?
C8 C9 C10 C11 -175.3(2) . . . . ?
C15 N2 C11 C12 1.4(3) . . . . ?
C15 N2 C11 C10 179.4(2) . . . . ?
N1 C10 C11 N2 168.4(2) . . . . ?
C9 C10 C11 N2 -13.4(3) . . . . ?
N1 C10 C11 C12 -13.5(3) . . . . ?
C9 C10 C11 C12 164.7(2) . . . . ?
N2 C11 C12 C13 -0.1(4) . . . . ?
C10 C11 C12 C13 -178.1(2) . . . . ?
C11 C12 C13 C14 -0.2(4) . . . . ?
C12 C13 C14 C15 -0.7(3) . . . . ?
C11 N2 C15 C14 -2.3(3) . . . . ?
C11 N2 C15 C16 177.50(19) . . . . ?
C13 C14 C15 N2 2.1(4) . . . . ?
C13 C14 C15 C16 -177.8(2) . . . . ?
C20 N3 C16 C17 0.5(3) . . . . ?
C20 N3 C16 C15 -179.5(2) . . . . ?
N2 C15 C16 N3 -178.1(2) . . . . ?
C14 C15 C16 N3 1.7(3) . . . . ?
N2 C15 C16 C17 1.9(3) . . . . ?
C14 C15 C16 C17 -178.3(2) . . . . ?
N3 C16 C17 C18 -0.8(4) . . . . ?
C15 C16 C17 C18 179.2(2) . . . . ?
C16 C17 C18 C19 1.3(4) . . . . ?
C17 C18 C19 C20 -1.4(4) . . . . ?
C16 N3 C20 C19 -0.6(3) . . . . ?
C16 N3 C20 C21 178.9(2) . . . . ?
C18 C19 C20 N3 1.1(4) . . . . ?
C18 C19 C20 C21 -178.4(2) . . . . ?
N3 C20 C21 C22 -79(7) . . . . ?
C19 C20 C21 C22 101(7) . . . . ?
C20 C21 C22 Si2 3(11) . . . . ?
C23 Si2 C22 C21 121(5) . . . . ?
C24 Si2 C22 C21 -118(5) . . . . ?
C25 Si2 C22 C21 1(5) . . . . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21147076
