Efforts toward Distorted Spiropentanes
Kuan-Jen Su; Jean-Luc Mieusset; Vladimir B. Arion; Wolfgang Knoll; Lothar Brecker; Udo H. Brinker; Journal of Organic Chemistry 75 (2010) 7494–7497; doi:10.1021/jo1017298

data_4025787
_publ_section_title
;
 Efforts toward Distorted Spiropentanes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7494
_journal_page_last               7497
_journal_paper_doi               10.1021/jo1017298
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C16 H14 Br4'
_chemical_formula_sum            'C16 H14 Br4'
_chemical_formula_weight         525.91
_chemical_name_systematic
; 
1,5-Bis-(2,2'-dibromocyclopropyl)-2,4-divinylnenzene
;
_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                83.730(5)
_cell_angle_beta                 85.515(5)
_cell_angle_gamma                87.424(5)
_cell_formula_units_Z            4
_cell_length_a                   6.5274(6)
_cell_length_b                   14.3878(15)
_cell_length_c                   18.4199(19)
_cell_measurement_reflns_used    2562
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.19
_cell_measurement_theta_min      2.52
_cell_volume                     1713.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.1440
_diffrn_reflns_av_sigmaI/netI    0.1491
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35174
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    9.385
_exptl_absorpt_correction_T_max  0.8345
_exptl_absorpt_correction_T_min  0.2555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.488
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0788P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1656
_reflns_number_gt                3263
_reflns_number_total             6203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo1017298_si_001_4.cif
_cod_data_source_block           kusu386
_cod_database_code               4025787