Synthesis of Cyclo[18]carbon via Debromination of C<sub>18</sub>Br<sub>6</sub>.
Scriven, Lorel M.; Kaiser, Katharina; Schulz, Fabian; Sterling, Alistair J.; Woltering, Steffen L.; Gawel, Przemyslaw; Christensen, Kirsten E.; Anderson, Harry L.; Gross, Leo; Journal of the American Chemical Society 142 (2020) 12921–12924; doi:10.1021/jacs.0c05033

data_4135114
_publ_section_title
;
 Synthesis of Cyclo[18]carbon via Debromination of
 C<sub>18</sub>Br<sub>6</sub>.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12921
_journal_page_last               12924
_journal_paper_doi               10.1021/jacs.0c05033
_journal_volume                  142
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 Br6'
_chemical_formula_sum            'C18 Br6'
_chemical_formula_weight         695.62
_chemical_melting_point          ?
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2020-04-14
_audit_creation_method           'CRYSTALS_ver_14.61_build_7491 '
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.6885(16)
_cell_length_b                   13.647(4)
_cell_length_c                   12.5084(11)
_cell_measurement_reflns_used    408
_cell_measurement_temperature    150
_cell_measurement_theta_max      47.67
_cell_measurement_theta_min      5.20
_cell_volume                     3702.3(12)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXT '
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1301
_diffrn_reflns_av_sigmaI/netI    0.1830
_diffrn_reflns_av_unetI/netI     0.099
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            906
_diffrn_reflns_theta_full        50.225
_diffrn_reflns_theta_max         50.225
_diffrn_reflns_theta_min         5.212
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.648
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.27
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            clear_intense_red
_exptl_crystal_density_diffrn    2.496
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.87
_refine_diff_density_min         -1.61
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 169 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9687
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         902
_refine_ls_number_restraints     219
_refine_ls_R_factor_all          0.2032
_refine_ls_R_factor_gt           0.1297
_refine_ls_shift/su_max          0.0000615
_refine_ls_shift/su_mean         0.0000117
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.20P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3720
_refine_ls_wR_factor_gt          0.2958
_refine_ls_wR_factor_ref         0.3720
_reflns_limit_h_max              21
_reflns_limit_h_min              0
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              -11
_reflns_number_gt                460
_reflns_number_total             906
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   7.04
_oxford_diffrn_Wilson_scale      550.43
_oxford_refine_ls_r_factor_ref   0.2032
_oxford_refine_ls_scale          0.04987(7)
_oxford_reflns_number_all        902
_oxford_structure_analysis_title '7256-c Fdd2-cba'
_cod_data_source_file            ja0c05033_si_002.cif
_cod_data_source_block           C18Br6
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 4135114.cif.

 Adding full bibliography for 4135114.cif.
;
_cod_original_cell_volume        3702(1)
_cod_original_sg_symbol_H-M      'F d d 2 '
_cod_database_code               4135114
_oxford_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_refine_ls_r_factor_all   0.2032
_oxford_refine_ls_wr_factor_all  0.3720
_oxford_hooft_y                  -0.1(3)
_oxford_bijvoet_difference       -0.1(2)
_oxford_refined_flack_x          0.2(4)