Synthesis and structure of 1′,4′-diphenyl-1a,1′,4′,4′′,5′′,9b-hexahydro-2′′H-dispiro[cyclopropa[l]phenanthrene-1,2′-[1,4]epoxynaphthalene-3′,3′′-thiophene]
Wen, Yuewei; Thamattoor, Dasan M.; Acta Crystallographica Section E Crystallographic Communications 81 (2025) –; doi:10.1107/S2056989025004104

data_2023511
_publ_section_title
;
 Synthesis and structure of
 1&#x2032;,4&#x2032;-diphenyl-1a,1&#x2032;,4&#x2032;,4&#x2032;&#x2032;,5&#x2032;&#x2032;,9b-hexahydro-2&#x2032;&#x2032;H-dispiro[cyclopropa[l]phenanthrene-1,2&#x2032;-[1,4]epoxynaphthalene-3&#x2032;,3&#x2032;&#x2032;-thiophene]
;
_journal_coeditor_code           HB8140
_journal_issue                   6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989025004104
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac          'C39 H30 O S'
_chemical_formula_moiety         'C39 H30 O S'
_chemical_formula_sum            'C39 H30 O S'
_chemical_formula_weight         546.69
_chemical_name_systematic
1',4'-Diphenyl-1a,1',4',4'',5'',9b-hexahydro-2''<i>H</i>-dispiro[cyclopropa[l]phenanthrene-1,2'-[1,4]epoxynaphthalene-3',3''-thiophene]
_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
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7205)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.121(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2352(14)
_cell_length_b                   14.3939(14)
_cell_length_c                   19.120(3)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.57
_cell_volume                     2788.6(6)
_computing_cell_refinement
;
SAINT-Plus V8.40B (Bruker, 2021)
;
_computing_data_collection
;
APEX4 Ver. 2021.10-0 (Bruker, 2021)
;
_computing_data_reduction
;
SAINT-Plus V8.40B (Bruker, 2021)
;
_computing_molecular_graphics
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Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
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Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
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_computing_structure_refinement
;
<i>SHELXL</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173
_diffrn_detector
'Charge-integrating Pixel Array (CPA) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST ECO diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34580
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.394
_diffrn_reflns_theta_min         2.795
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.706
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0449P)^2^+1.7735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                4424
_reflns_number_total             5692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8140.cif
_cod_data_source_block           I
_cod_database_code               2023511
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.985
_shelx_hkl_checksum              64153
_shelx_res_checksum              18462