Novel hydrazone derivatives of 7-hydroxy-3',3'-dimethyl-3'<i>H</i>-spiro[chromene-2,1'-isobenzofuran]-8-carbaldehyde
Bulanov, Antony; Shcherbakov, Igor N.; Popov, Leonid D.; Shasheva, E. Y.; Belikov, P. A.; Starikova, Zoya A.; Acta Crystallographica Section C 67 (2011) o85–o88; doi:10.1107/S0108270111002836

data_2018014
_publ_section_title
;
 Novel hydrazone derivatives of
 7-hydroxy-3',3'-dimethyl-3'<i>H</i>-spiro[chromene-2,1'-isobenzofuran]-8-carbaldehyde
;
_journal_coeditor_code           LG3049
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o85
_journal_page_last               o88
_journal_paper_doi               10.1107/S0108270111002836
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C27 H25 N3 O3 S'
_chemical_formula_moiety         'C27 H25 N3 O3 S'
_chemical_formula_sum            'C27 H25 N3 O3 S'
_chemical_formula_weight         471.56
_chemical_melting_point          463
_chemical_name_common
;
<i>N</i>-benzyl-2-[(7-hydroxy-3',3'-dimethyl-3'<i>H</i>-spiro[chromene-2,1'-
isobenzofuran]-8-yl)methylidene]hydrazinecarbothioamide
;
_chemical_name_systematic
;
1-benzyl-3-({7'-hydroxy-3,3-dimethylspiro[2-benzofuran-1,2'-chromene]-8'-
ylmethylidene}amino)thiourea
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.020(4)
_cell_angle_beta                 83.192(4)
_cell_angle_gamma                77.714(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4023(14)
_cell_length_b                   9.4893(15)
_cell_length_c                   15.210(3)
_cell_measurement_reflns_used    209
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      3
_cell_volume                     1176.1(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1998)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       '\w scans at different fixed \f positions'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_sigmaI/netI    0.1085
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9676
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.353
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.1334
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                2089
_reflns_number_total             4139
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lg3049.cif
_cod_data_source_block           I
_cod_original_cell_volume        1176.1(3)
_cod_database_code               2018014
_cod_database_fobs_code          2018014