Two androst-5-ene derivatives: 16-[4-(3-chloropropoxy)-3-methoxybenzylidene]-17-oxoandrost-5-en-3β-ol and 16-[3-methoxy-4-(2-pyrrolidin-1-ylethoxy)benzylidene]-3β-pyrrolidinoandrost-5-en-17β-ol monohydrate
Thamotharan, S.; Parthasarathi, V.; Gupta, Ranju; Guleria, Sheetal; Jindal, D. P.; Linden, Anthony; Acta Crystallographica Section C 60 (2004) o75–o78; doi:10.1107/S0108270103025605

data_2013853
_publ_section_title
;Two androst-5-ene derivatives:
 16-[4-(3-chloropropoxy)-3-methoxybenzylidene]-17-oxoandrost-5-en-3\b-ol and
 16-[3-methoxy-4-(2-pyrrolidin-1-ylethoxy)benzylidene]-3\b-pyrrolidinoandrost-5-en-17\b-ol
 monohydrate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o75
_journal_page_last               o78
_journal_paper_doi               10.1107/S0108270103025605
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C37 H54 N2 O3 , H2 O'
_chemical_formula_moiety         'C37 H54 N2 O3 , H2 O'
_chemical_formula_sum            'C37 H56 N2 O4'
_chemical_formula_weight         592.86
_chemical_melting_point          483
_chemical_name_systematic
;
16-[3-methoxy-4-(2-pyrrolidin-1-ylethoxy)benzylidene]-
3\b-pyrrolidinoandrost-5-en-17\b-ol monohydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 99.6510(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.42190(10)
_cell_length_b                   32.4115(5)
_cell_length_c                   8.09810(10)
_cell_measurement_reflns_used    3313
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.0
_cell_volume                     1661.71(4)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1999)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w scans with \k offsets'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'Nonius FR591 sealed tube generator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_av_sigmaI/netI    0.035
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            36139
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.0757
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.22
_refine_ls_extinction_coef       0.017(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         3299
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.046
_refine_ls_R_factor_gt           0.037
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.1844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.086
_refine_ls_wR_factor_ref         0.092
_reflns_number_gt                2865
_reflns_number_total             3302
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1678.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2013853
_cod_database_fobs_code          2013853