Thermal dimerization of [n]cumulenes (n = 5, 7, 9)
Dominik Wendinger; Johanna A. Januszewski; Frank Hampel; Rik R. Tykwinski; Chem.Commun. 51 (2015) 14877–; doi:10.1039/C5cc05679a

data_7117858
_publ_section_title
;
 Thermal dimerization of [n]cumulenes (n = 5, 7, 9)
;
_journal_name_full               Chem.Commun.
_journal_page_first              14877
_journal_paper_doi               10.1039/C5cc05679a
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C72 H56, 2(C H2 Cl2)'
_chemical_formula_sum            'C74 H60 Cl4'
_chemical_formula_weight         1091.02
_chemical_name_systematic
;
 ? 
;
_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             2013-04-12
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2015-05-26 deposited with the CCDC.
2015-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                104.011(5)
_cell_angle_beta                 90.739(4)
_cell_angle_gamma                104.207(4)
_cell_formula_units_Z            1
_cell_length_a                   9.7822(5)
_cell_length_b                   12.5174(6)
_cell_length_c                   12.6361(8)
_cell_measurement_reflns_used    4130
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      61.8770
_cell_measurement_theta_min      3.7550
_cell_volume                     1451.01(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      173.000(10)
_diffrn_detector_area_resol_mean 10.6144
_diffrn_measured_fraction_theta_full 0.9837
_diffrn_measured_fraction_theta_max 0.9527
_diffrn_measurement_details
;
  1 omega  -86.00  -34.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -30.0000 52

  2 omega  -26.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -150.0000 98

  3 omega    7.00   42.00   1.0000    2.7900
omega____ theta____ kappa____ phi______ frames
    -       82.7293  -30.0000 -150.0000 35

  4 omega   23.00  122.00   1.0000    2.7900
omega____ theta____ kappa____ phi______ frames
    -       82.7293 -125.0000  -30.0000 99

  5 omega   57.00  155.00   1.0000    2.7900
omega____ theta____ kappa____ phi______ frames
    -       82.7293   30.0000 -150.0000 98

  6 omega   54.00  149.00   1.0000    2.7900
omega____ theta____ kappa____ phi______ frames
    -       82.7293   30.0000  120.0000 95

  7 omega   10.00   99.00   1.0000    2.7900
omega____ theta____ kappa____ phi______ frames
    -       82.7293  -45.0000  -60.0000 89

  8 omega   56.00   98.00   1.0000    2.7900
omega____ theta____ kappa____ phi______ frames
    -       82.7293 -125.0000  120.0000 42

  9 omega   19.00  115.00   1.0000    2.7900
omega____ theta____ kappa____ phi______ frames
    -       82.7293  -77.0000  120.0000 96
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0620895000
_diffrn_orient_matrix_UB_12      -0.1021834000
_diffrn_orient_matrix_UB_13      -0.0460138000
_diffrn_orient_matrix_UB_21      -0.0545971000
_diffrn_orient_matrix_UB_22      -0.0052352000
_diffrn_orient_matrix_UB_23      -0.1165242000
_diffrn_orient_matrix_UB_31      0.1404025000
_diffrn_orient_matrix_UB_32      0.0821681000
_diffrn_orient_matrix_UB_33      -0.0137175000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6450
_diffrn_reflns_theta_full        61.96
_diffrn_reflns_theta_max         61.96
_diffrn_reflns_theta_min         3.77
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.181
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             572
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.2648
_exptl_crystal_size_mid          0.1574
_exptl_crystal_size_min          0.1046
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0812P)^2^+0.6294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1474
_reflns_number_gt                3828
_reflns_number_total             4350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc05679a2.cif
_cod_data_source_block           dw07
_cod_original_cell_volume        1451.00(14)
_cod_database_code               7117858
_chemical_oxdiff_formula         'C36 H28'
_reflns_odcompleteness_completeness 98.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86