Synthesis and Phosphatase Inhibitory Activity of 3-Alkynylestrones and their Derivatives
Ivanov, Anton; Boldt, Sebastian; Nisa, Zaib un; Shah, Syed; Ehlers, Peter; Villinger, Alexander; Schneider, Gyula; Wölfling, János; Rahman, Qamar; Iqbal, Jamshed; Langer, Peter; RSC Adv.  (2016) –; doi:10.1039/C5RA25558A

data_7223886
_publ_section_title
;
 Synthesis and Phosphatase Inhibitory Activity of 3-Alkynylestrones and
 their Derivatives
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA25558A
_journal_year                    2016
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C29 H30 O'
_chemical_formula_sum            'C29 H30 O'
_chemical_formula_weight         394.53
_chemical_name_systematic
3-[[4-(n-propyl)phenyl]ethynyl]estra-1,3,5(10)-trien-17-one
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-10-30 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.599(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.9542(5)
_cell_length_b                   7.8665(6)
_cell_length_c                   21.0214(15)
_cell_measurement_reflns_used    3446
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.70
_cell_measurement_theta_min      2.77
_cell_volume                     1144.49(15)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16543
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.766
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 1486 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -1.2(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         6282
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+0.0040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1369
_reflns_Friedel_coverage         0.770
_reflns_friedel_fraction_full    0.935
_reflns_friedel_fraction_max     0.878
_reflns_number_gt                4335
_reflns_number_total             6282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra25558a2.cif
_cod_data_source_block           av_sb22
_cod_database_code               7223886
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2013-4
_shelx_res_checksum              40913