Photo- and Thermal-Induced Multistructural Transformation of 2-Phenylazolyl Chelate Boron Compounds
Ying-Li Rao; Hazem Amarne; Leanne D. Chen; Matthew L. Brown; Nicholas J. Mosey; Suning Wang; Journal of the American Chemical Society 135 (2013) 3407–3410; doi:10.1021/ja400917r

data_4119424
_publ_section_title
;
 Photo- and Thermal-Induced Multistructural Transformation of
 2-Phenylazolyl Chelate Boron Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3407
_journal_page_last               3410
_journal_paper_doi               10.1021/ja400917r
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C31 H30 B N S'
_chemical_formula_weight         459.44
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 127.814(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.898(5)
_cell_length_b                   32.238(17)
_cell_length_c                   8.756(4)
_cell_measurement_reflns_used    2444
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      20.50
_cell_measurement_theta_min      2.41
_cell_volume                     3099(3)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1016
_diffrn_reflns_av_sigmaI/netI    0.1442
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16179
_diffrn_reflns_theta_full        27.23
_diffrn_reflns_theta_max         27.23
_diffrn_reflns_theta_min         1.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  0.9763
_exptl_absorpt_correction_T_min  0.9534
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.985
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
'4 disordered toluene molecules were removed from the lattice'
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(11)
_refine_ls_extinction_coef       0.0120(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6647
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1777
_reflns_number_gt                3708
_reflns_number_total             6647
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400917r_si_001.cif
_cod_data_source_block           yr40b
_cod_original_cell_volume        3099(2)
_cod_database_code               4119424