Crystal structure and solvent-dependent behaviours of 3-amino-1,6-diethyl-2,5,7-trimethyl-4,4-diphenyl-3a,4a-diaza-4-bora-<i>s</i>-indacene
Yang, Lijing; Drew, Brett; Yalagala, Ravi Shekar; Chaviwala, Rameez; Simionescu, Razvan; Lough, Alan J.; Yan, Hongbin; Acta Crystallographica Section E 73 (2017) 378–382; doi:10.1107/S2056989017002213

data_2242225
_publ_section_title
;
 Crystal structure and solvent-dependent behaviours of
 3-amino-1,6-diethyl-2,5,7-trimethyl-4,4-diphenyl-3a,4a-diaza-4-bora-<i>s</i>-indacene
;
_journal_coeditor_code           SJ5520
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              378
_journal_page_last               382
_journal_paper_doi               10.1107/S2056989017002213
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C28 H32 B N3'
_chemical_formula_moiety         'C28 H32 B N3'
_chemical_formula_sum            'C28 H32 B N3'
_chemical_formula_weight         421.37
_chemical_name_systematic
3-Amino-1,6-diethyl-2,5,7-trimethyl-4,4-diphenyl-3a,4a-diaza-4-bora-<i>s</i>-indacene
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 109.557(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4938(7)
_cell_length_b                   11.5325(8)
_cell_length_c                   11.3739(9)
_cell_measurement_reflns_used    4278
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.43
_cell_volume                     1173.45(15)
_computing_cell_refinement
;
APEX2 (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      147(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10457
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         1.900
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       plate
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.186
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1500 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al</i>, 2013)
;
_refine_ls_abs_structure_Flack   -1.3(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5032
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0464P)^2^+0.0459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                4054
_reflns_number_total             5032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5520sup1.cif
_cod_data_source_block           I
_cod_database_code               2242225
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.995
_shelx_hkl_checksum              80457
_shelx_res_checksum              48736
_cod_database_fobs_code 2242225