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_7052233
_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 . C4 H10 O1 '
_chemical_formula_sum            'C38 H40 O9'
_chemical_formula_weight         640.70
_chemical_name_common
;2,3-bis(4-benzyloxy-3-methoxy-benzilidene)-succinic acid
buthanol solvate
;
_chemical_name_systematic
;
2,3-bis(4-benzyloxy-3-methoxy-benzilidene)-succinic acid
buthanol 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                101.68(1)
_cell_angle_beta                 106.69(1)
_cell_angle_gamma                96.91(1)
_cell_formula_units_Z            2
_cell_length_a                   10.929(1)
_cell_length_b                   11.708(1)
_cell_length_c                   15.385(2)
_cell_measurement_reflns_used    2297
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      44.0
_cell_measurement_theta_min      6.0
_cell_volume                     1812.9(4)
_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_publication_material  'SHELXL-97 (Sheldrick, 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 0.949
_diffrn_measured_fraction_theta_max 0.949
_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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14403
_diffrn_reflns_theta_full        58.04
_diffrn_reflns_theta_max         58.04
_diffrn_reflns_theta_min         5.25
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1986)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.167
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.0007(4)
_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   0.787
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         4790
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      0.802
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0577
_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^)+(0.1127P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                1862
_reflns_number_total             4790
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b515266f.txt
_cod_data_source_block           fulgen1b
_cod_original_cell_volume        1812.9(3)
_cod_database_code               7052233