Synthesis and Photophysical Properties of Two Strongly Fluorescent Bis(diquinaldinatoalumino)-9-silafluorenes
Pusztai, Erika; Albright, Haley; Cai, Yuanjing; Hu, Rongrong; West, Robert; Tang, Ben Zhong; Guzei, Ilia A.; Organometallics 32 (2013) 6871–; doi:10.1021/om4005803

data_4081818
_publ_section_title
;
 Synthesis and Photophysical Properties of Two Strongly Fluorescent
 Bis(diquinaldinatoalumino)-9-silafluorenes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6871
_journal_paper_doi               10.1021/om4005803
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C52 H40 Al2 N4 O6 Si, C7 H8'
_chemical_formula_sum            'C59 H48 Al2 N4 O6 Si'
_chemical_formula_weight         991.06
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2013-10-14
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                72.641(11)
_cell_angle_beta                 87.604(17)
_cell_angle_gamma                71.992(13)
_cell_formula_units_Z            2
_cell_length_a                   10.088(4)
_cell_length_b                   14.811(7)
_cell_length_c                   18.210(7)
_cell_measurement_reflns_used    7616
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.558
_cell_measurement_theta_min      2.178
_cell_volume                     2465.9(18)
_computing_cell_refinement       'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 Ver. 2013.2-0 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008-2013)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.09
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48199
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.607
_diffrn_reflns_theta_min         1.173
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1153 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.9244.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         15062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.6526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1239
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10116
_reflns_number_total             15062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om4005803_si_002.cif
_cod_data_source_block           west312
_cod_original_cell_volume        2465.8(18)
_cod_database_code               4081818
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.969
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C16(H16),
 C17(H17), C18(H18), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28), C29(H29),
  C30(H30), C31(H31), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40),
 C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C55(H55), C56(H56), C57(H57),
  C58(H58), C59(H59)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C33(H33A,H33B,H33C), C43(H43A,H43B,
 H43C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              65840
_shelx_hkl_checksum              58829