Dialkoxybenzo[j]fluoranthenes: synthesis, structures, photophysical properties, and optical waveguide application
Li, Xiao-Jun; Li, Meng; Yao, Wei; Lu, Hai-Yan; Zhao, YongSheng; Chen, Chuan-Feng; RSC Advances 5 (2015) 18609–; doi:10.1039/C4RA17112H

data_7235729
_publ_section_title
;
 Dialkoxybenzo[j]fluoranthenes: synthesis, structures, photophysical
 properties, and optical waveguide application
;
_journal_issue                   24
_journal_name_full               'RSC Advances'
_journal_page_first              18609
_journal_paper_doi               10.1039/C4RA17112H
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C28 H28 O2'
_chemical_formula_sum            'C28 H28 O2'
_chemical_formula_weight         396.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2014-12-02 deposited with the CCDC.
2015-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                98.39(3)
_cell_angle_beta                 94.84(3)
_cell_angle_gamma                99.51(3)
_cell_formula_units_Z            4
_cell_length_a                   8.1661(16)
_cell_length_b                   13.473(3)
_cell_length_c                   20.342(4)
_cell_measurement_reflns_used    6164
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4779
_cell_measurement_theta_min      1.5532
_cell_volume                     2170.1(8)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2013)'
_computing_structure_solution
;
'XS (Sheldrick, 2013)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0887
_diffrn_orient_matrix_UB_12      -0.0826
_diffrn_orient_matrix_UB_13      -0.0305
_diffrn_orient_matrix_UB_21      0.0437
_diffrn_orient_matrix_UB_22      0.0429
_diffrn_orient_matrix_UB_23      -0.0455
_diffrn_orient_matrix_UB_31      0.0338
_diffrn_orient_matrix_UB_32      0.0155
_diffrn_orient_matrix_UB_33      0.0334
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_unetI/netI     0.0917
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21365
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.844
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.146
_refine_diff_density_max         1.353
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         9810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1327
_refine_ls_R_factor_gt           0.1046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0838P)^2^+1.3402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2319
_refine_ls_wR_factor_ref         0.2511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7402
_reflns_number_total             9810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra17112h2.cif
_cod_data_source_block           sa3265
_cod_database_code               7235729
_shelxl_version_number           2013-4
_diffrn_number_total             9820
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21A(H21A,H21B), C22A(H22A,H22B), C23A(H23A,H23B), C25A(H25A,H25B), C26A(H26A,
 H26B), C27A(H27A,H27B), C21(H21C,H21D), C22(H22C,H22D), C23(H23C,H23D),
 C25(H25C,H25D), C26(H26C,H26D), C27(H27C,H27D)
2.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C7A(H7A), C12A(H12A), C13A(H13A),
 C17A(H17A), C19A(H19A), C20A(H20A), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7),
 C12(H12), C13(H13), C17(H17), C19(H19), C20(H20)
2.c Idealised Me refined as rotating group:
 C24A(H24A,H24B,H24C), C28A(H28A,H28B,H28C), C24(H24D,H24E,H24F), C28(H28D,
 H28E,H28F)
;
_shelx_res_checksum              75510
_shelx_hkl_checksum              49434