Synthetic Studies toward Polytwistane Hydrocarbon Nanorods.
Olbrich, Martin; Mayer, Peter; Trauner, Dirk; The Journal of organic chemistry 80 (2015) 2042–2055; doi:10.1021/jo502618g

data_4030410
_publ_section_title
;
 Synthetic Studies toward Polytwistane Hydrocarbon Nanorods.
;
_journal_issue                   4
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2042
_journal_page_last               2055
_journal_paper_doi               10.1021/jo502618g
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C29 H30 Br P Pd'
_chemical_formula_sum            'C29 H30 Br P Pd'
_chemical_formula_weight         595.85
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_block_code                Pd_Br_PPh3_C11H15_po051_trauner
_audit_creation_date
;
'Wed Mar 23 10:43:31 2011'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             23-Mar-11
_cell_angle_alpha                90.00
_cell_angle_beta                 97.985(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3791(3)
_cell_length_b                   9.9376(2)
_cell_length_c                   19.0528(5)
_cell_measurement_reflns_used    10142
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.2498
_cell_measurement_theta_min      4.2281
_cell_volume                     2508.63(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_structure_refinement
;
Sheldrick, G. M. (2008).
<i>Acta Cryst.</i> A<b>64</b>, 112--122.
;
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega   12.00   43.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4494   77.0000 -150.0000 31

  2 omega   19.00   50.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4494   77.0000   90.0000 31

  3 omega  -44.00  -13.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4494   77.0000  -30.0000 31

  4 omega   17.00   48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4494   77.0000  -30.0000 31

  5 omega  -12.00   94.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3869   77.0000   60.0000 106

  6 omega  -12.00   94.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3869   77.0000  -60.0000 106

  7 omega  -12.00   89.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3869   77.0000 -180.0000 101

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0450278211
_diffrn_orient_matrix_UB_12      0.0274230135
_diffrn_orient_matrix_UB_13      0.0185802842
_diffrn_orient_matrix_UB_21      0.0256597319
_diffrn_orient_matrix_UB_22      -0.0609849459
_diffrn_orient_matrix_UB_23      -0.0047373723
_diffrn_orient_matrix_UB_31      0.0133476982
_diffrn_orient_matrix_UB_32      0.0247827184
_diffrn_orient_matrix_UB_33      -0.0323253616
_diffrn_radiation_collimation    '0.5 mm collimator'
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18759
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         4.24
_diffrn_source_current           40_mA
_diffrn_source_power             2.00_kW
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50_kV
_exptl_absorpt_coefficient_mu    2.411
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.57766(6)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0208
_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/[\s^2^(Fo^2^)+(0.0229P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0446
_reflns_number_gt                4027
_reflns_number_total             5085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo502618g_si_002.cif
_cod_data_source_block           compound25
_cod_depositor_comments
'Adding full bibliography for 4030407--4030418.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4030410