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_4025786
_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         'c18 H14 Br8, C H2 Cl2'
_chemical_formula_sum            'C19 H16 Br8 Cl2'
_chemical_formula_weight         954.50
_chemical_name_systematic
; 
1,2,4,5-Tetrakis-(2,2-dibromocyclopropyl)-benzene 
dichloromethane solvate
;
_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                 105.572(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6247(5)
_cell_length_b                   20.0130(9)
_cell_length_c                   12.1491(4)
_cell_measurement_reflns_used    2638
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.65
_cell_measurement_theta_min      2.48
_cell_volume                     2488.47(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.1415
_diffrn_reflns_av_sigmaI/netI    0.1062
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43829
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    13.114
_exptl_absorpt_correction_T_max  0.6220
_exptl_absorpt_correction_T_min  0.1790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.927
_refine_diff_density_min         -2.672
_refine_diff_density_rms         0.271
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4504
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0519P)^2^+24.8429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1334
_reflns_number_gt                2876
_reflns_number_total             4504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo1017298_si_001_3.cif
_cod_data_source_block           kusu305
_cod_database_code               4025786