symm-Tetramethylenecyclooctane: En Route to Polyspirocycles.
Averina, Elena B.; Sedenkova, Kseniya N.; Bakhtin, Stanislav G.; Grishin, Yuri K.; Kutateladze, Andrei G.; Roznyatovsky, Vitaly A.; Rybakov, Victor B.; Butov, Gennady M.; Kuznetsova, Tamara S.; Zefirov, Nikolay S.; The Journal of organic chemistry 79 (2014) 8163–8170; doi:10.1021/jo501380y

data_4029886
_publ_contact_author             'Dr Victor B. Rybakov'
_publ_section_title
;
 symm-Tetramethylenecyclooctane: En Route to Polyspirocycles.
;
_journal_issue                   17
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8163
_journal_page_last               8170
_journal_paper_doi               10.1021/jo501380y
_journal_volume                  79
_journal_year                    2014
_chemical_formula_moiety         'C16 H16 Br8'
_chemical_formula_sum            'C16 H16 Br8'
_chemical_formula_weight         847.57
_chemical_melting_point_gt       462
_chemical_melting_point_lt       463
_chemical_name_systematic
; 
 1,1,6,6,10,10,14,14--Octabromotetraspiro[2.1.25.1.29.1.213.13]hexadecane
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.151(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8295(4)
_cell_length_b                   18.6950(6)
_cell_length_c                   11.8467(6)
_cell_measurement_reflns_used    20182
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      3.04
_cell_volume                     2128.21(16)
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0615
_diffrn_reflns_av_sigmaI/netI    0.2064
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5525
_diffrn_reflns_theta_full        28.90
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    15.073
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Light Yellow'
_exptl_crystal_density_diffrn    2.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1568
_exptl_crystal_preparation       'C H Cl3'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.577
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         5525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.577
_refine_ls_R_factor_all          0.1341
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0035P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0387
_refine_ls_wR_factor_ref         0.0525
_reflns_number_gt                2125
_reflns_number_total             5525
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo501380y_si_002.cif
_cod_data_source_block           aver55
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4029886--4029887.cif.
;
_cod_original_cell_volume        2128.21(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4029886