Designed synthesis of “L” shaped 17-halo-aryl-ethynyl steroids
Ochoa, María Eugenia; Aguilar-Granda, Andrés; Ramirez-Montes, Pedro I.; Barba, Victor; López, Yliana; Santillan, Rosa; Farfán, Norberto; CrystEngComm 18 (2016) 6830–; doi:10.1039/C6CE01056C

data_7225989
_publ_section_title
;
 Designed synthesis of &#x201C;L&#x201D; shaped 17-halo-aryl-ethynyl
 steroids
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              6830
_journal_paper_doi               10.1039/C6CE01056C
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C26  H27  O2  I1  Cl0'
_chemical_formula_sum            'C26 H27 I O2'
_chemical_formula_weight         498.37
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_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             2016-02-25T15:17:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-03-10 deposited with the CCDC.
2016-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3430(2)
_cell_length_b                   17.0390(4)
_cell_length_c                   20.654(5)
_cell_measurement_reflns_used    13767
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     2584.2(6)
_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_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.983
_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
_diffrn_orient_matrix_UB_11      0.061039
_diffrn_orient_matrix_UB_12      -0.027495
_diffrn_orient_matrix_UB_13      -0.036862
_diffrn_orient_matrix_UB_21      0.112136
_diffrn_orient_matrix_UB_22      -0.006766
_diffrn_orient_matrix_UB_23      0.026903
_diffrn_orient_matrix_UB_31      -0.047406
_diffrn_orient_matrix_UB_32      -0.051406
_diffrn_orient_matrix_UB_33      0.016175
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       -1000000
_diffrn_reflns_limit_h_min       1000000
_diffrn_reflns_limit_k_max       -1000000
_diffrn_reflns_limit_k_min       1000000
_diffrn_reflns_limit_l_max       -1000000
_diffrn_reflns_limit_l_min       1000000
_diffrn_reflns_number            5816
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.944
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.906
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 1619 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+1.8403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1393
_reflns_Friedel_coverage         0.756
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                4632
_reflns_number_total             5816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01056c2.cif
_cod_data_source_block           san529
_cod_depositor_comments
'Adding full bibliography for 7225988--7225998.cif.'
_cod_database_code               7225989
_shelx_estimated_absorpt_t_min   0.744
_shelx_estimated_absorpt_t_max   0.806
_platon_squeeze_void_probe_radius 1.20