Pentaleno[1,2-a:4,5']diacenaphthylenes: Uniquely Stabilized Pentalene Derivatives.
Yuan, Bingxin; Zhuang, Junpeng; Kirmess, Kristopher M.; Bridgmohan, Chelsea N.; Whalley, Adam C.; Wang, Lichang; Plunkett, Kyle N.; The Journal of organic chemistry 81 (2016) 8312–8318; doi:10.1021/acs.joc.6b01480

data_4037101
_publ_contact_author
; 
Kyle N. Plunkett
Southern Illinois University
1245 Lincoln Dr.
Carbondale, IL  62901
;
_publ_section_title
;
 Pentaleno[1,2-a:4,5']diacenaphthylenes: Uniquely Stabilized Pentalene
 Derivatives.
;
_journal_issue                   18
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8312
_journal_page_last               8318
_journal_paper_doi               10.1021/acs.joc.6b01480
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C40 H22'
_chemical_formula_sum            'C40 H22'
_chemical_formula_weight         502.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 110.788(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8411(10)
_cell_length_b                   6.8502(5)
_cell_length_c                   14.7405(11)
_cell_measurement_reflns_used    5272
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.17
_cell_measurement_theta_min      3.93
_cell_volume                     1212.22(16)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/5, 
(Bruker, 2012 & 2014) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-7 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX-2014-7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_id  cd47wsa
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9487
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.375
_diffrn_reflns_theta_min         3.932
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.97639
_exptl_absorpt_correction_T_min  0.93057
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             524
_exptl_crystal_id                cd47wsa
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-3 0 4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.0080(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+0.6924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1827
_reflns_number_total             2219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b01480_si_002.cif
_cod_data_source_block           cd47wsa
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4037101
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.896
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              94743
_shelx_hkl_checksum              74556