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_4030416
_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         'C24 H27 O3 P'
_chemical_formula_sum            'C24 H27 O3 P'
_chemical_formula_weight         394.443
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_block_code                C24H27O3P_qo101_trauner
_audit_creation_date
;
'Wed Jun 20 06:43:31 2012'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             20-Jun-12
_cell_angle_alpha                90.040(4)
_cell_angle_beta                 81.463(5)
_cell_angle_gamma                85.164(4)
_cell_formula_units_Z            2
_cell_length_a                   7.2398(4)
_cell_length_b                   9.5416(4)
_cell_length_c                   14.6831(9)
_cell_measurement_reflns_used    3480
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.4391
_cell_measurement_theta_min      4.1584
_cell_volume                     999.40(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega -103.00  -47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  148.0000  154.0000 56

  2 omega  -80.00  -33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000 -150.0000 47

  3 omega    3.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   38.0000 -120.0000 95

  4 omega   34.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000   90.0000 69

  5 omega  -37.00   53.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -38.0000   60.0000 90

  6 omega    4.00   40.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000   90.0000 36

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0845636000
_diffrn_orient_matrix_UB_12      -0.0034490000
_diffrn_orient_matrix_UB_13      -0.0315713000
_diffrn_orient_matrix_UB_21      -0.0522372000
_diffrn_orient_matrix_UB_22      0.0103494000
_diffrn_orient_matrix_UB_23      -0.0370230000
_diffrn_orient_matrix_UB_31      0.0026965000
_diffrn_orient_matrix_UB_32      0.0738079000
_diffrn_orient_matrix_UB_33      0.0043780000
_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  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8998
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         4.17
_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    0.160
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.31078(12)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         6024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0485P)^2^+0.2722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                5051
_reflns_number_total             6024
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo502618g_si_002.cif
_cod_data_source_block           compound39
_cod_depositor_comments
'Adding full bibliography for 4030407--4030418.cif.'
_cod_database_code               4030416