Crystalline Hybrid Polyphenylene Macromolecules from Octaalkynylsilsesquioxanes, Crystal Structures, and a Potential Route to 3-D Graphenes
Roll, Mark F.; Kampf, Jeffrey W.; Laine, Richard M.; Macromolecules 44 (2011) 3425–; doi:10.1021/ma200081q

data_1501790
_publ_section_title
;
 Crystalline Hybrid Polyphenylene Macromolecules from
 Octaalkynylsilsesquioxanes, Crystal Structures, and a Potential Route to
 3-D Graphenes
;
_journal_issue                   9
_journal_name_full               Macromolecules
_journal_page_first              3425
_journal_paper_doi               10.1021/ma200081q
_journal_volume                  44
_journal_year                    2011
_chemical_formula_moiety
;

                         'C368 H296 O12 Si8, 9(C8 H10), C7 H8, (solvent)'

;
_chemical_formula_sum            'C447 H394 O12 Si8'
_chemical_formula_weight         6182.34
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.6146(19)
_cell_length_b                   32.6146(19)
_cell_length_c                   41.178(5)
_cell_measurement_reflns_used    9674
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      20.60
_cell_measurement_theta_min      2.21
_cell_volume                     43802(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART-APEX'
_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      85(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0828
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            511019
_diffrn_reflns_theta_full        20.76
_diffrn_reflns_theta_max         20.76
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_correction_T_min  0.9764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

  Blessing, R. Acta Cryst. (1995) A51 33-38.

  Sheldrick, G.  SADABS (Version 2008/1) Bruker AXS area

  detector absorption and other corrections, University of

  Gottingen, Germany 2008.

;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.937
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             13136
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2514
_refine_ls_number_reflns         22627
_refine_ls_number_restraints     1717
_refine_ls_restrained_S_all      1.979
_refine_ls_R_factor_all          0.1385
_refine_ls_R_factor_gt           0.1193
_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^)+(0.1000P)^2^+2.1667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3056
_refine_ls_wR_factor_ref         0.3139
_reflns_number_gt                17779
_reflns_number_total             22627
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ma200081q_si_004.cif
_cod_data_source_block           whpb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P4/n
_cod_database_code               1501790