Phosphorus and silicon-bridged stilbenes: synthesis and optoelectronic properties.
Zhou, Yang; Yang, Shuai; Li, Jun; He, Gufeng; Duan, Zheng; Mathey, Francois; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18308–18312; doi:10.1039/c6dt03489f

data_7040970
_publ_section_title
;
 Phosphorus and silicon-bridged stilbenes: synthesis and optoelectronic
 properties.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18308
_journal_page_last               18312
_journal_paper_doi               10.1039/c6dt03489f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C22 H19 O P Si'
_chemical_formula_sum            'C22 H19 O P Si'
_chemical_formula_weight         358.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2014-09-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-09-18 deposited with the CCDC.
2016-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                84.434(3)
_cell_angle_beta                 76.892(3)
_cell_angle_gamma                77.143(4)
_cell_formula_units_Z            4
_cell_length_a                   10.2464(4)
_cell_length_b                   12.4270(6)
_cell_length_c                   17.6262(7)
_cell_measurement_reflns_used    7025
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      72.2780
_cell_measurement_theta_min      4.3580
_cell_volume                     2128.54(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -72.00  -38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000 -150.0000 34

  2 omega  -77.00  -52.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -30.0000 25

  3 omega  -29.00   -2.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000   30.0000 27

  4 omega   27.00   61.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000   30.0000 34

  5 omega  -73.00  -36.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000    0.0000 37

  6 omega   -2.00   37.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -120.0000 39

  7 omega   37.00   88.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000  -60.0000 51

  8 omega   41.00  111.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -125.0000 -180.0000 70

  9 omega   40.00   66.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   37.0000  -60.0000 26

 10 omega   30.00   72.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000  -90.0000 42

 11 omega    8.00   65.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000    0.0000 57

 12 omega   13.00  110.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   19.0000   90.0000 97

 13 omega   13.00   74.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000  150.0000 61

 14 omega   32.00  125.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   37.0000  150.0000 93

 15 omega  128.00  178.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   60.0000 50

 16 omega   89.00  115.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   60.0000 26

 17 omega   39.00   64.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -90.0000 25

 18 omega   42.00   98.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  120.0000 56

 19 omega   93.00  178.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000 -150.0000 85

 20 omega   68.00  114.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -90.0000 46

 21 omega   40.00  105.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -60.0000 65

 22 omega   92.00  178.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  150.0000 86

 23 omega   42.00   87.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -180.0000 45

 24 omega  111.00  139.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000   30.0000 28

 25 omega   48.00   81.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000   30.0000 33

 26 omega   41.00   98.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   30.0000 57

 27 omega   44.00   95.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -60.0000 51

 28 omega   60.00  103.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -180.0000 43

 29 omega   62.00  106.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   90.0000 44

 30 omega   39.00   64.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -180.0000 25

 31 omega   70.00  115.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   60.0000 45

 32 omega   93.00  174.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   90.0000 81

 33 omega  -77.00  -32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000   60.0000 45

 34 omega  -69.00   21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -180.0000 90

 35 omega  -69.00   21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -90.0000 90

 36 omega   26.00  114.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000 -180.0000 88
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0446266000
_diffrn_orient_matrix_UB_12      0.1095666000
_diffrn_orient_matrix_UB_13      -0.0302874000
_diffrn_orient_matrix_UB_21      -0.0847778000
_diffrn_orient_matrix_UB_22      0.0542914000
_diffrn_orient_matrix_UB_23      0.0755846000
_diffrn_orient_matrix_UB_31      0.1253714000
_diffrn_orient_matrix_UB_32      -0.0354328000
_diffrn_orient_matrix_UB_33      0.0379782000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15415
_diffrn_reflns_theta_full        67.07
_diffrn_reflns_theta_max         67.07
_diffrn_reflns_theta_min         3.65
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.718
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
 ?
;
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         7602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0414
_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/[\s^2^(Fo^2^)+(0.0730P)^2^+0.0682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                6273
_reflns_number_total             7602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt03489f3.cif
_cod_data_source_block           201408174
_cod_depositor_comments
'Adding full bibliography for 7040970--7040971.cif.'
_cod_original_cell_volume        2128.52(15)
_cod_database_code               7040970
_chemical_oxdiff_formula         C20H20N4P1Si1
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C14(H14),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C1'(H1'), C2'(H2'), C3'(H3'),
  C4'(H4'), C11'(H11'), C12'(H12'), C13'(H13'), C14'(H14'), C18'(H18'),
 C19'(H19'), C20'(H20'), C21'(H21'), C22'(H22')
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C15'(H15D,H15E,H15F), C16'(H16D,
 H16E,H16F)
;
_olex2_submission_special_instructions 'No special instructions were received'