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_7117857
_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         'C76 H56'
_chemical_formula_sum            'C76 H56'
_chemical_formula_weight         969.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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
_audit_creation_date             2015-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-29 deposited with the CCDC.
2015-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.2323(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.2177(3)
_cell_length_b                   9.01016(14)
_cell_length_c                   21.3998(4)
_cell_measurement_reflns_used    4167
_cell_measurement_temperature    172.9(3)
_cell_measurement_theta_max      63.5230
_cell_measurement_theta_min      5.3340
_cell_volume                     3094.80(10)
_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    '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      172.9(3)
_diffrn_detector_area_resol_mean 10.6144
_diffrn_measured_fraction_theta_full 0.784
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -86.00  -35.00   1.0000   27.9500
omega____ theta____ kappa____ phi______ frames
    -       -1.3659 -178.0000   30.0000 51

  2 omega  -20.00   41.00   1.0000   27.9500
omega____ theta____ kappa____ phi______ frames
    -        1.3659   77.0000 -120.0000 61

  3 omega   60.00  152.00   1.0000  111.8000
omega____ theta____ kappa____ phi______ frames
    -       85.9553   45.0000 -150.0000 92

  4 omega   15.00   91.00   1.0000  111.8000
omega____ theta____ kappa____ phi______ frames
    -       85.9553  -30.0000 -150.0000 76

  5 omega   59.00  158.00   1.0000  111.8000
omega____ theta____ kappa____ phi______ frames
    -       85.9553   30.0000  120.0000 99

  6 omega   21.00   89.00   1.0000  111.8000
omega____ theta____ kappa____ phi______ frames
    -       85.9553  -94.0000 -120.0000 68
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0751563000
_diffrn_orient_matrix_UB_12      0.0179214000
_diffrn_orient_matrix_UB_13      -0.0524012000
_diffrn_orient_matrix_UB_21      -0.0559274000
_diffrn_orient_matrix_UB_22      -0.0801809000
_diffrn_orient_matrix_UB_23      0.0416367000
_diffrn_orient_matrix_UB_31      -0.0210462000
_diffrn_orient_matrix_UB_32      0.1499042000
_diffrn_orient_matrix_UB_33      0.0284968000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_laue_measured_fraction_full 0.784
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7901
_diffrn_reflns_point_group_measured_fraction_full 0.784
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         58.916
_diffrn_reflns_theta_min         5.335
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'metallic brownish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.1367
_exptl_crystal_size_mid          0.0871
_exptl_crystal_size_min          0.0167
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4392
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1291P)^2^+0.6424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.1947
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                3760
_reflns_number_total             4392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc05679a2.cif
_cod_data_source_block           dw06
_cod_original_cell_volume        3094.81(10)
_cod_database_code               7117857
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C38 H28'
_reflns_odcompleteness_completeness 98.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_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. Restrained distances
 C37-C36 \\sim C37A-C32
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C37A) = Uanis(C37)
4. Others
 Sof(H36)=Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(1)
 Sof(H32)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C22(H22), C23(H23), C24(H24),
 C25(H25), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43),
  C44(H44), C45(H45)
5.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C37A(H37D,H37E,
 H37F), C47(H47A,H47B,H47C)
;
_olex2_date_sample_data_collection 2013-03-19
_olex2_date_sample_submission    1363561200
_olex2_exptl_crystal_mounting_method 'mounted on a loop'
_olex2_submission_special_instructions 'No special instructions were received'