Synthesis, crystal structures and phase transformation of the new solid-state forms of tetrandrine
Zhou, Zhengzheng; Tong, Henry H. Y.; Li, Liang; Shek, Fanny L. Y.; Lv, Yang; Zheng, Ying; RSC Adv. 4 (2014) 62586–; doi:10.1039/C4RA10457A

data_7218822
_publ_section_title
;
 Synthesis, crystal structures and phase transformation of the new
 solid-state forms of tetrandrine
;
_journal_issue                   107
_journal_name_full               'RSC Adv.'
_journal_page_first              62586
_journal_paper_doi               10.1039/C4RA10457A
_journal_volume                  4
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_sum            'C82 H95 N4 O14'
_chemical_formula_weight         1360.62
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           1
_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_date             2014-04-08T23:06:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.296(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.7432(5)
_cell_length_b                   9.9123(3)
_cell_length_c                   19.3410(6)
_cell_measurement_temperature    100(10)
_cell_volume                     3587.39(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(10)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25210
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    0.69
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.26
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1454
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         12057
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+0.7131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1171
_reflns_number_gt                10877
_reflns_number_total             12057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra10457a1.cif
_cod_data_source_block           02268a
_cod_original_cell_volume        3587.38(18)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7218822