Temperature-Driven Isosymmetric Reversible Phase Transition of the Hormone Estradiol 17β Valerate
Ellena, Javier; de Paula, Karina; de Melo, Cristiane C.; da Silva, Cecília C. P.; Bezerra, Beatriz P.; Venâncio, Tiago; Ayala, Alejandro P.; Crystal Growth & Design 14 (2014) 5700–; doi:10.1021/cg500974r

data_4512201
_publ_section_title
;
 Temperature-Driven Isosymmetric Reversible Phase Transition of the
 Hormone Estradiol 17\b Valerate
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5700
_journal_paper_doi               10.1021/cg500974r
_journal_volume                  14
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C23  H32  O3'
_chemical_formula_sum            'C23 H32 O3'
_chemical_formula_weight         356.49
_chemical_name_common
estra-1,3,5(10)-triene-3,17-diol(17?)-17-pentanoate
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   constr
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2014-06-14T11:44:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.619(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3706(2)
_cell_length_b                   19.8583(5)
_cell_length_c                   13.9888(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     1.54178
_cell_volume                     2047.39(9)
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.92
_diffrn_measured_fraction_theta_max 0.942
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.92
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25841
_diffrn_reflns_point_group_measured_fraction_full 0.853
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.566
_diffrn_reflns_theta_min         4.453
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.468
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.29
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 2053 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.14(10)
_refine_ls_extinction_coef       0.0021(5)
_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   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     474
_refine_ls_number_reflns         6321
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.069
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0914P)^2^+0.4469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1649
_reflns_number_gt                5226
_reflns_number_total             6321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg500974r_si_002.cif
_cod_data_source_block           E2v298K
_cod_depositor_comments
'Adding full bibliography for 4512201--4512202.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4512201
_shelx_estimated_absorpt_t_min   0.771
_shelx_estimated_absorpt_t_max   0.967