Structural and conformational study of two solvates of a fulgenic acid derivative
Giannellini, Valerio; Bambagiotti-Alberti, Massimo; Bruni, Bruno; Di Vaira, Massimo; New Journal of Chemistry 30 (2006) 647–; doi:10.1039/b515266f

data_7052232
_publ_section_title
;
 Structural and conformational study of two solvates of a fulgenic acid
 derivative
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              647
_journal_paper_doi               10.1039/b515266f
_journal_volume                  30
_journal_year                    2006
_chemical_formula_moiety         'C34 H30 O8 . C1 H4 O1 '
_chemical_formula_sum            'C35 H34 O9'
_chemical_formula_weight         598.62
_chemical_name_common
;2,3-bis(4-benzyloxy-3-methoxy-benzilidene)-succinic acid
methanol solvate
;
_chemical_name_systematic
;
2,3-bis(4-benzyloxy-3-methoxy-benzilidene)-succinic acid
methanol solvate
;
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.297(3)
_cell_angle_beta                 74.559(3)
_cell_angle_gamma                77.321(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6859(4)
_cell_length_b                   10.7325(4)
_cell_length_c                   14.5858(5)
_cell_measurement_reflns_used    8905
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      55.0
_cell_measurement_theta_min      6.0
_cell_volume                     1525.75(10)
_computing_cell_refinement       'CrysAlisCCD (Oxford Diffraction, 2001)'
_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2001)'
_computing_data_reduction        'CrysAlisRED (Oxford Diffraction, 2001)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Oxford Diffraction, Excalibur PX Ultra, CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16190
_diffrn_reflns_theta_full        65.47
_diffrn_reflns_theta_max         65.47
_diffrn_reflns_theta_min         4.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1986)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.0046(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         4927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                3705
_reflns_number_total             4927
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b515266f.txt
_cod_data_source_block           fulgen1a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7052232