4,4-Difluoro-2,3;5,6-bis(tetramethylene)-4-bora-3a,4a-diaza-<i>s</i>-indacene (LD540)
Salorinne, Kirsi; Tero, Tiia-Riikka; Lahtinen, Tanja; Acta Crystallographica Section E 70 (2014) o74–; doi:10.1107/S1600536813033448

data_2239137
_publ_section_title
;
 4,4-Difluoro-2,3;5,6-bis(tetramethylene)-4-bora-3a,4a-diaza-<i>s</i>-indacene
 (LD540)
;
_journal_coeditor_code           VM2201
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o74
_journal_paper_doi               10.1107/S1600536813033448
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C18 H21 B F2 N2'
_chemical_formula_moiety         'C18 H21 B F2 N2'
_chemical_formula_sum            'C18 H21 B F2 N2'
_chemical_formula_weight         314.18
_chemical_name_common
;
2,2-difluoro-12-methyl-1\l^5^,3-diaza-2\l^4^-
borapentacyclo[11.7.0.0^3,11^.0^4,9^.0^15,20^]icosa-
1(20),4(9),10,12,14-pentaen-1-ylium, LD540
;
_chemical_name_systematic
;
4,4-Difluoro-2,3;5,6-bis(tetramethylene)-4-bora-3a,4a-diaza-<i>s</i>-indacene
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 111.271(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8836(4)
_cell_length_b                   16.4670(10)
_cell_length_c                   11.4865(6)
_cell_measurement_reflns_used    2349
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      62.389
_cell_measurement_theta_min      0.883
_cell_volume                     1565.85(15)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Bruker, 2004)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type
'Nonius KappaCCD diffractometer with APEXII detector'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7413
_diffrn_reflns_theta_full        67.683
_diffrn_reflns_theta_max         63.307
_diffrn_reflns_theta_min         4.928
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.839612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            'green red'
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.303
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0626P)^2^+0.2776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1245
_reflns_number_gt                1902
_reflns_number_total             2511
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            vm2201sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1565.84(15)
_cod_database_code               2239137
_cod_database_fobs_code          2239137
_shelx_hkl_checksum              23064
_shelx_res_checksum              92150
_shelxl_version_number           .2013