Versatile solid modifications of icariin: structure, properties and form transformation
Jia, Lina; Zhang, Qi; Wang, Jian-Rong; Mei, Xuefeng; CrystEngComm 17 (2015) 7500–; doi:10.1039/C5CE01422K

data_7221965
_publ_section_title
;
 Versatile solid modifications of icariin: structure, properties and form
 transformation
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              7500
_journal_paper_doi               10.1039/C5CE01422K
_journal_volume                  17
_journal_year                    2015
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C35.5 H47 O15.5'
_chemical_formula_weight         720.22
_chemical_name_common            Icariin
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-17 deposited with the CCDC.
2015-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.7994(7)
_cell_length_b                   23.0446(16)
_cell_length_c                   31.541(2)
_cell_measurement_temperature    296(2)
_cell_volume                     7122.7(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APXII-CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0951
_diffrn_reflns_av_sigmaI/netI    0.1602
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            30317
_diffrn_reflns_theta_full        24.86
_diffrn_reflns_theta_max         24.86
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    0.106
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3060
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1.4(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         11879
_refine_ls_number_restraints     2266
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1952
_refine_ls_R_factor_gt           0.0926
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0929P)^2^+0.6534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.2247
_reflns_number_gt                5824
_reflns_number_total             11879
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01422k2.cif
_cod_data_source_block           mo_2014503_0m
_cod_depositor_comments
'Adding full bibliography for 7221958--7221966.cif.'
_cod_original_cell_volume        7122.6(9)
_cod_database_code               7221965