Triple Structural Transition below Room Temperature in the Antifilarial Drug Diethylcarbamazine Citrate
da Silva, Cecilia C. P.; Martins, Felipe T.; Honorato, Sara B.; Boechat, Núbia; Ayala, Alejandro P.; Ellena, Javier; Crystal Growth & Design 10 (2010) 3094–; doi:10.1021/cg100212q

data_4501670
_publ_section_title
;
 Triple Structural Transition below Room Temperature in the Antifilarial
 Drug Diethylcarbamazine Citrate
;
_journal_issue                   7
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3094
_journal_paper_doi               10.1021/cg100212q
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C10 H22 N3 O, C6 H7 O7'
_chemical_formula_sum            'C16 H29 N3 O8'
_chemical_formula_weight         391.42
_chemical_name_systematic
;
 diethylcarbamazine citrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.033(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.4386(7)
_cell_length_b                   10.1644(2)
_cell_length_c                   14.0536(3)
_cell_measurement_reflns_used    8189
_cell_measurement_temperature    235(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      2.910
_cell_volume                     3904.39(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      235(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0920
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14878
_diffrn_reflns_theta_full        26.84
_diffrn_reflns_theta_max         26.84
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         8234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1442
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.1993
_reflns_number_gt                4343
_reflns_number_total             8234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg100212q_si_001.cif
_cod_data_source_block           DECCitrate_235K
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4501670