Synthesis of Hybrid Masked Triyne-Phenylene Axial Rods Containing (E)-β-Chlorovinylsilanes in the π-Conjugated Framework
Michael D. Weller; Benson M. Kariuki; Liam R. Cox; Journal of Organic Chemistry 74 (2009) 7898–7907; doi:10.1021/jo901766p

data_4024931
_publ_section_title
;
Synthesis of Hybrid Masked Triyne-Phenylene Axial Rods Containing
(E)-\b-Chlorovinylsilanes in the \p-Conjugated Framework
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7898
_journal_page_last               7907
_journal_paper_doi               10.1021/jo901766p
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C50 H44 Br4 Cl2 Si2'
_chemical_formula_sum            'C50 H44 Br4 Cl2 Si2'
_chemical_formula_weight         1091.57
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.583(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5108(3)
_cell_length_b                   20.4120(6)
_cell_length_c                   11.4447(3)
_cell_measurement_reflns_used    3553
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      70.87
_cell_measurement_theta_min      4.33
_cell_volume                     2452.93(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.946
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15757
_diffrn_reflns_theta_full        70.87
_diffrn_reflns_theta_max         70.87
_diffrn_reflns_theta_min         4.33
_exptl_absorpt_coefficient_mu    5.719
_exptl_absorpt_correction_T_max  0.4614
_exptl_absorpt_correction_T_min  0.3942
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.368
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0689P)^2^+3.8321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1542
_reflns_number_gt                3553
_reflns_number_total             4467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo901766p_si_003.cif
_cod_data_source_block           mdw329m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4024931