Synthesis and structure of large difluoromethylene containing alicycles by ring closing metathesis (RCM).
Skibiński, Maciej; Urbina-Blanco, César A; Slawin, Alexandra M. Z.; Nolan, Steven P.; O'Hagan, David; Organic & biomolecular chemistry 11 (2013) 8209–8213; doi:10.1039/c3ob42062k

data_7153216
_publ_section_title
;
 Synthesis and structure of large difluoromethylene containing alicycles
 by ring closing metathesis (RCM).
;
_journal_issue                   47
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8209
_journal_page_last               8213
_journal_paper_doi               10.1039/c3ob42062k
_journal_volume                  11
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H34 S4'
_chemical_formula_sum            'C20 H34 S4'
_chemical_formula_weight         402.73
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 97.633(15)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   7.101(5)
_cell_length_b                   36.72(3)
_cell_length_c                   8.124(5)
_cell_measurement_reflns_used    4285
_cell_measurement_temperature    125
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.22
_cell_volume                     2100(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r5'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r5'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      125
_diffrn_detector_area_resol_mean 28.944
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8541
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.334
_diffrn_reflns_theta_min         1.109
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             872.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.990
_refine_diff_density_min         -1.010
_refine_ls_abs_structure_details ' Flack x determined using 1453 quotients'
_refine_ls_abs_structure_Flack   -0.01(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3976
_refine_ls_number_restraints     2
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1318P)^2^+1.2396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2222
_reflns_number_gt                3684
_reflns_number_total             3976
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c3ob42062k.txt
_cod_data_source_block           8b
_cod_database_code               7153216