Synthesis, characterisation and optical spectroscopy of diynes and poly-ynes containing derivatised fluorenes in the backbone
Muhammad S. Khan; Muna R. A. Al-Mandhary; Mohammed K. Al-Suti; Birte Ahrens; Mary F. Mahon; Louise Male; Paul R. Raithby; Clare E. Boothby; Anna Köhler; Dalton Trans.  (2003) 74–84; doi:10.1039/b208963g

data_7012223
_publ_section_title
;
 Synthesis, characterisation and optical spectroscopy of diynes and
 poly-ynes containing derivatised fluorenes in the backbone
;
_journal_issue                   1
_journal_name_full               'Dalton Trans.'
_journal_page_first              74
_journal_page_last               84
_journal_paper_doi               10.1039/b208963g
_journal_year                    2003
_chemical_formula_sum            'C39 H58 Si2'
_chemical_formula_weight         583.03
_chemical_name_systematic        'Compound 2a'
_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                68.2370(10)
_cell_angle_beta                 89.3960(10)
_cell_angle_gamma                83.8980(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1696(2)
_cell_length_b                   14.1102(2)
_cell_length_c                   14.4029(3)
_cell_measurement_reflns_used    17456
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     1907.63(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
_computing_molecular_graphics    ORTEP-99
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DirDif-99 (Beurskens, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '528 2 degree images'
_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  0.0744
_diffrn_reflns_av_sigmaI/netI    0.0883
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46744
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  0.9885
_exptl_absorpt_correction_T_min  0.9750
_exptl_absorpt_correction_type   'Semi Empirical'
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_density_diffrn    1.015
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Tablet
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         8639
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1798
_refine_ls_R_factor_gt           0.0976
_refine_ls_shift/su_max          0.086
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
[1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/
[\s^2^(Fo^2^)+0.0000+0.3272*P+(0.1886P)^2^+1.0000sin\q/\l]
where P == 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2862
_refine_ls_wR_factor_ref         0.3348
_reflns_number_gt                4313
_reflns_number_total             8639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208963g.txt
_cod_data_source_block           h01prr9
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012223