Polymerization of acetylene: polyynes, but not carbyne
Prenzel, Dominik; Kirschbaum, Rolf W.; Chalifoux, Wesley A.; McDonald, Robert; Ferguson, Michael J.; Drewello, Thomas; Tykwinski, Rik R.; Organic Chemistry Frontiers 4 (2017) 668–; doi:10.1039/C6QO00648E

data_1553588
_publ_section_title
;
 Polymerization of acetylene: polyynes, but not carbyne
;
_journal_issue                   5
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              668
_journal_paper_doi               10.1039/C6QO00648E
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C45 H64, C H2 Cl2'
_chemical_formula_sum            'C46 H66 Cl2'
_chemical_formula_weight         689.88
_chemical_name_systematic
'3,3,3-tris(3,5-di-t-butyl)prop-1-yne, dichloromethane solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-09-30 deposited with the CCDC.
2016-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.6212(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4263(9)
_cell_length_b                   10.2668(9)
_cell_length_c                   40.789(4)
_cell_measurement_reflns_used    5254
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.18
_cell_volume                     4366.0(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            31531
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         1.997
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8924
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_description       prism
_exptl_crystal_F_000             1504
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2'
_exptl_crystal_size_max          0.590
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         8298
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0598P)^2^+2.0474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6236
_reflns_number_total             8298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qo00648e2.cif
_cod_data_source_block           Tr-H1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1553588
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              94228
_shelx_hkl_checksum              15131
_shelx_fab_checksum              67230