Photoisomerization of 1-Phenyl-2-(pyridin-2-yl)indole BMes2: The Dark Isomer
Amarne, Hazem; Baik, Chul; Wang, Rui-Yao; Wang, Suning; Organometallics 30 (2011) 665–; doi:10.1021/om101111p

data_4064064
_publ_section_title
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 Photoisomerization of 1-Phenyl-2-(pyridin-2-yl)indole BMes2: The Dark
 Isomer
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_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              665
_journal_paper_doi               10.1021/om101111p
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C37 H35 B N2'
_chemical_formula_weight         518.48
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 111.807(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4517(17)
_cell_length_b                   13.3461(11)
_cell_length_c                   15.9493(15)
_cell_measurement_reflns_used    1008
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      15.18
_cell_measurement_theta_min      2.19
_cell_volume                     3053.7(5)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.2517
_diffrn_reflns_av_sigmaI/netI    0.3106
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25137
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.9994
_exptl_absorpt_correction_T_min  0.9968
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
Difference electron density maps revealed the presence of disordered 
lattice solvate molecules, which were ultimately modeled through the
use of the SQUEEZE subroutine of the PLATON software suite. PLATON 
Reference: P. v.d. Sluis & A.L. Spek. Acta Cryst. (1990), A46, 194. 
Two solvent accessible voids per lattice were found. Each has a 
total volume of 145 A3 and contributing a total of 4.2 electrons. 
Since the crystal was obtained in pure hexane, 
the void was thus assigned to a half of hexane, which 
contribute 0.5x50 = 25 electrons, and ocuppy about 60 A3 in space. 
The larger volume and the smaller number of the electron of the void 
may be a result of the disorder. The contributions have been included 
in all derived crystal quantities 
although the precise composition of the lattice solvate is somewhat 
speculative.
;
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5366
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      0.878
_refine_ls_R_factor_all          0.3241
_refine_ls_R_factor_gt           0.1122
_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^)+(0.1040P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2367
_refine_ls_wR_factor_ref         0.3252
_reflns_number_gt                1262
_reflns_number_total             5366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101111p_si_002.cif
_cod_data_source_block           baik13a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4064064