Synthesis and luminescent properties of lewis base-appended borafluorenes.
Berger, Christopher J.; He, Gang; Merten, Christian; McDonald, Robert; Ferguson, Michael J.; Rivard, Eric; Inorganic chemistry 53 (2014) 1475–1486; doi:10.1021/ic402408t

data_4337317
_publ_section_title
;
 Synthesis and luminescent properties of lewis base-appended
 borafluorenes.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1475
_journal_page_last               1486
_journal_paper_doi               10.1021/ic402408t
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
'C26 H28 B Br N4, 0.5(C4 H8 O), 0.33(C H2 Cl2)'
_chemical_formula_sum            'C28.33 H32.67 B Br Cl0.67 N4 O0.5'
_chemical_formula_weight         551.60
_chemical_name_common            10
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.3286(4)
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   29.9685(7)
_cell_length_b                   12.7445(3)
_cell_length_c                   43.8064(10)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.96
_cell_measurement_theta_min      2.22
_cell_volume                     16726.6(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            66493
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.473
_diffrn_reflns_theta_min         1.629
_exptl_absorpt_coefficient_mu    1.564
_exptl_absorpt_correction_T_max  0.8258
_exptl_absorpt_correction_T_min  0.6946
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       prism
_exptl_crystal_F_000             6864
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.264
_exptl_crystal_size_min          0.182
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as disordered or
partial-occupancy solvent tetrahydrofuran oxygen or carbon atoms were
unsuccessful.  The data were corrected for disordered electron density
through use of the SQUEEZE procedure (Sluis, P. van der; Spek, A. L.
Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON (Spek,
A. L. Acta Crystallogr. 1990, A46, C34; Spek, A. L. J. Appl. Cryst.
2003, 36, 7-13.  PLATON - a multipurpose crystallographic tool.
Utrecht University, Utrecht, The Netherlands).  A total
solvent-accessible void volume of 2100.4 cubic Angstroms with a total
electron count of 448 (consistent with 12 molecules of solvent
tetrahydrofuran, or one-half THF molecule per formula unit of the
5,5-bis(4-dimethylaminopyridine)-5H-dibenzo[b,d]borol-5-ylium ion) was
found in the unit cell.
;
_refine_diff_density_max         1.510
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         17236
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.1058P)^2^+23.1038P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.1996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11962
_reflns_number_total             17236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402408t_si_002.cif
_cod_data_source_block           riv1352
_cod_original_formula_sum        'C28.33 H32.67 B Br Cl0.67 N4 O0.50'
_cod_database_code               4337317
_shelx_estimated_absorpt_t_min   0.644
_shelx_estimated_absorpt_t_max   0.764
_shelxl_version_number           2013-2
_shelx_res_checksum              62305
_shelx_hkl_checksum              15526