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_2018015
_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 H24 N2 O4, C3 H6 O'
_chemical_formula_moiety         'C27 H24 N2 O4, C3 H6 O'
_chemical_formula_sum            'C30 H30 N2 O5'
_chemical_formula_weight         498.56
_chemical_melting_point          436
_chemical_name_common
;
<i>N</i>'-[(7-Hydroxy-3',3'-dimethyl-3'<i>H</i>-spiro[chromene-2,1'-
isobenzofuran]-8-yl)methylidene]-4-methylbenzohydrazide acetone monosolvate
;
_chemical_name_systematic
;
<i>N</i>'-{7'-hydroxy-3,3-dimethyl-3<i>H</i>-spiro[2-benzofuran-1,2'-
chromene]-8'-ylmethylidene}-4-methylbenzohydrazide acetone monosolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.265(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.591(2)
_cell_length_b                   17.272(5)
_cell_length_c                   17.569(5)
_cell_measurement_reflns_used    294
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     2602.7(12)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0924
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20745
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         4568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0096P)^2^+1.9500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                2752
_reflns_number_total             4568
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lg3049.cif
_cod_data_source_block           II
_cod_original_cell_volume        2602.6(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2018015
_cod_database_fobs_code          2018015