Synthesis and Structure Activity Relationship of Organometallic Steroidal Androgen Derivatives
Top, Siden; Thibaudeau, Céline; Vessières, Anne; Brulé, Emilie; Le Bideau, Franck; Joerger, Jean-Michel; Plamont, Marie-Aude; Samreth, Soth; Edgar, Alan; Marrot, Jérôme; Herson, Patrick; Jaouen, Gérard; Organometallics 28 (2009) 1414–; doi:10.1021/om800698y

data_4068322
_publ_section_title
;
 Synthesis and Structure Activity Relationship of Organometallic Steroidal
 Androgen Derivatives
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1414
_journal_paper_doi               10.1021/om800698y
_journal_volume                  28
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C31 H40 Fe1 O2.5'
_chemical_formula_sum            'C31 H40 Fe O2.5'
_chemical_formula_weight         508.50
_space_group_IT_number           79
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.967(3)
_cell_length_b                   25.967(4)
_cell_length_c                   8.1833(11)
_cell_measurement_reflns_used    166
_cell_measurement_temperature    250
_cell_measurement_theta_max      21
_cell_measurement_theta_min      3
_cell_volume                     5517.9(13)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      250
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10829
_diffrn_reflns_theta_full        25.205
_diffrn_reflns_theta_max         30.006
_diffrn_reflns_theta_min         1.568
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.22
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.16
_refine_diff_density_min         -0.62
_refine_ls_abs_structure_details 'Flack (1983), 1504 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0840
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         3466
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.000641
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 2.03 0.142E-01 1.50 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0670
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0569
_reflns_limit_h_max              25
_reflns_limit_h_min              -25
_reflns_limit_k_max              36
_reflns_limit_k_min              0
_reflns_limit_l_max              7
_reflns_limit_l_min              -11
_reflns_number_gt                3466
_reflns_number_total             5546
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0536
_oxford_reflns_number_all        5542
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            om800698y_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_refine_ls_hydrogen_treatment' value 'refu' changed to
'refU' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'I 4 '
_cod_original_formula_sum        'C31 H40 Fe1 O2.5'
_cod_database_code               4068322