A step toward polytwistane: synthesis and characterization of C2-symmetric tritwistane.
Olbrich, Martin; Mayer, Peter; Trauner, Dirk; Organic & biomolecular chemistry 12 (2014) 108–112; doi:10.1039/c3ob42152j

data_7153656
_publ_section_title
;
 A step toward polytwistane: synthesis and characterization of
 C2-symmetric tritwistane.
;
_journal_issue                   1
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              108
_journal_page_last               112
_journal_paper_doi               10.1039/c3ob42152j
_journal_volume                  12
_journal_year                    2014
_chemical_formula_moiety         'C14 H18 Br2'
_chemical_formula_sum            'C14 H18 Br2'
_chemical_formula_weight         346.101
_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                C14H18Br2_qo120_trauner
_audit_creation_date
;
'Tue Jul 17 10:26:40 2012'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             20-Jul-12
_cell_angle_alpha                90.00
_cell_angle_beta                 101.998(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0330(10)
_cell_length_b                   7.7467(6)
_cell_length_c                   12.4282(9)
_cell_measurement_reflns_used    1603
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.7784
_cell_measurement_theta_min      4.2016
_cell_volume                     1227.37(16)
_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 0.992
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_details
;
  1 omega  -93.00   11.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931  -77.0000  -30.0000 104

  2 omega  -52.00   53.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2306  -38.0000 -180.0000 105

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0275131000
_diffrn_orient_matrix_UB_12      -0.0543032000
_diffrn_orient_matrix_UB_13      0.0423444000
_diffrn_orient_matrix_UB_21      -0.0480216000
_diffrn_orient_matrix_UB_22      -0.0383463000
_diffrn_orient_matrix_UB_23      0.0056095000
_diffrn_orient_matrix_UB_31      0.0055893000
_diffrn_orient_matrix_UB_32      -0.0629553000
_diffrn_orient_matrix_UB_33      -0.0397625000
_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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4608
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         28.84
_diffrn_reflns_theta_min         4.21
_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    6.574
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41499
_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    1.8730(2)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0390
_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/[\s^2^(Fo^2^)+(0.0453P)^2^+0.2889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.1006
_reflns_number_gt                2166
_reflns_number_total             2708
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ob42152j.txt
_cod_data_source_block           qo120
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7153656