Synthesis of polyynes to model the sp-carbon allotrope carbyne.
Chalifoux, Wesley A.; Tykwinski, Rik R.; Nature chemistry 2 (2010) 967–971; doi:10.1038/nchem.828

data_1508130
_publ_section_title
;
 Synthesis of polyynes to model the sp-carbon allotrope carbyne.
;
_journal_issue                   11
_journal_name_full               'Nature chemistry'
_journal_page_first              967
_journal_page_last               971
_journal_paper_doi               10.1038/nchem.828
_journal_volume                  2
_journal_year                    2010
_chemical_formula_moiety         'C64 H84 Si, C6 H14'
_chemical_formula_sum            'C70 H98 Si'
_chemical_formula_weight         967.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                76.520(1)
_cell_angle_beta                 89.555(1)
_cell_angle_gamma                86.272(1)
_cell_formula_units_Z            2
_cell_length_a                   10.2575(7)
_cell_length_b                   14.6634(11)
_cell_length_c                   21.9595(16)
_cell_measurement_reflns_used    3789
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.00
_cell_measurement_theta_min      2.21
_cell_volume                     3205.0(4)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22875
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         0.95
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.9953
_exptl_absorpt_correction_T_min  0.9722
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.003
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as disordered or
partial-occupancy solvent hexane carbon atoms were unsuccessful.  The
data were corrected for disordered electron density through use of the
SQUEEZE procedure (Sluis, P. van der; Spek, A. L. Acta Crystallogr.
1990, A46, 194&#x0096;201) as implemented in PLATON (Spek, A.L. Acta
Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7&#x0096;13.
PLATON - a multipurpose crystallographic tool.  Utrecht University,
Utrecht, The Netherlands).  A total solvent-accessible void volume of
464 A3 with a total electron count of 108 (consistent with 2 molecules
of solvent hexane, or 1 molecule per formula unit of the
(C6H3tBu2)3C(CC)6SiMe3 molecule) was found in the unit cell.
;
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         11578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0968P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1675
_refine_ls_wR_factor_ref         0.1884
_reflns_number_gt                6600
_reflns_number_total             11578
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            nchem.828-s3.cif
_cod_data_source_block           3-6
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
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_cod_database_code               1508130