Crystal structure of <i>rac</i>-(3a'<i>R</i>,9a'<i>R</i>)-3a'-(indol-3-yl)-1',2',3',3a',4',9a'-hexahydrospiro[cyclopentane-1,9'-pentaleno[1,2-<i>b</i>]indole] <i>p</i>-xylene hemisolvate
Noland, Wayland E.; Worth, Matthew A.; Schneerer, Andrew K.; Paal, Courtney L.; Tritch, Kenneth J.; Acta Crystallographica Section E 71 (2015) 516–519; doi:10.1107/S2056989015007422

data_2240574
_publ_section_title
;
 Crystal structure of
 <i>rac</i>-(3a'<i>R</i>,9a'<i>R</i>)-3a'-(indol-3-yl)-1',2',3',3a',4',9a'-hexahydrospiro[cyclopentane-1,9'-pentaleno[1,2-<i>b</i>]indole]
 <i>p</i>-xylene hemisolvate
;
_journal_coeditor_code           SU5116
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              516
_journal_page_last               519
_journal_paper_doi               10.1107/S2056989015007422
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C26 H26 N2, 0.5C8 H10'
_chemical_formula_moiety         'C26 H26 N2, 0.5(C8 H10)'
_chemical_formula_sum            'C30 H31 N2'
_chemical_formula_weight         419.57
_chemical_melting_point          459
_chemical_name_common            I
_chemical_name_systematic
;
<i>rac</i>-(3a'<i>R</i>,9a'<i>R</i>)-3a'-(Indol-3-yl)-1',2',3',3a',4',9a'-\
hexahydrospiro[cyclopentane-1,9'-pentaleno[1,2-<i>b</i>]indole]
<i>p</i>-xylene hemisolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 114.7320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7618(7)
_cell_length_b                   29.450(2)
_cell_length_c                   9.6569(8)
_cell_measurement_reflns_used    2946
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.28
_cell_measurement_theta_min      2.42
_cell_volume                     2263.3(3)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015), enCIFer (Allen <i>et al.</i>,
2004), and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25883
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.423
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       Block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.371
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         5184
_refine_ls_number_restraints     321
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0542P)^2^+0.8656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                4102
_reflns_number_total             5184
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su5116sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2263.2(3)
_cod_database_code               2240574
_cod_database_fobs_code          2240574
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.991
_shelx_hkl_checksum              48600
_shelx_res_checksum              66681
_shelxl_version_number           2014/6