Synthesis of Air- and Moisture-Stable Dibenzogallepins: Control of Planarity of Seven-Membered Rings in Solid States by Coordination to Gallium Atoms
Matsumoto, Takuya; Takamine, Hirofumi; Tanaka, Kazuo; Chujo, Yoshiki; Organic Letters  (2015) 150304071945009–; doi:10.1021/acs.orglett.5b00489

data_1518778
_publ_section_title
;
 Synthesis of Air- and Moisture-Stable Dibenzogallepins: Control of
 Planarity of Seven-Membered Rings in Solid States by Coordination to
 Gallium Atoms
;
_journal_name_full               'Organic Letters'
_journal_page_first              150304071945009
_journal_paper_doi               10.1021/acs.orglett.5b00489
_journal_year                    2015
_chemical_formula_sum            'C32 H39 Ga'
_chemical_formula_weight         493.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.260(8)
_cell_angle_beta                 90.512(6)
_cell_angle_gamma                92.334(7)
_cell_formula_units_Z            2
_cell_length_a                   9.1296(6)
_cell_length_b                   10.8681(7)
_cell_length_c                   13.8864(10)
_cell_measurement_temperature    93(2)
_cell_volume                     1314.37(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12545
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.064
_exptl_absorpt_correction_T_max  0.8154
_exptl_absorpt_correction_T_min  0.7408
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.466
_refine_diff_density_min         -2.643
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1078P)^2^+2.2455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1940
_reflns_number_gt                4917
_reflns_number_total             5974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol5b00489_si_002.cif
_cod_data_source_block           ydkr
_cod_original_cell_volume        1314.37(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1518778