Palladium catalyzed synthesis of benzannulated steroid spiroketals.
Mayorquín-Torres, Martha C; González-Orozco, Juan Carlos; Flores-Álamo, Marcos; Camacho-Arroyo, Ignacio; Iglesias-Arteaga, Martín A; Organic & biomolecular chemistry 18 (2020) 725–737; doi:10.1039/c9ob02255d

data_7157270
_publ_section_title
;
 Palladium catalyzed synthesis of benzannulated steroid spiroketals.
;
_journal_issue                   4
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              725
_journal_page_last               737
_journal_paper_doi               10.1039/c9ob02255d
_journal_volume                  18
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_formula_sum            'C34 H52 O2'
_chemical_formula_weight         492.75
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_creation_date             2019-08-21T10:14:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-09-11 deposited with the CCDC.	2019-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.224(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.4753(5)
_cell_length_b                   8.3777(7)
_cell_length_c                   23.7615(17)
_cell_measurement_reflns_used    2293
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      73.48
_cell_measurement_theta_min      3.704
_cell_volume                     1476.27(19)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
          'Ortep-3 for Windows (Farrugia, 1997)'
      L. J. Farrugia, J. Appl. Crystallogr., 1997, 30, 565.
;
_computing_publication_material
;	
        'WinGX publication routines (Farrugia, 1999)'				 
	L. J. Farrugia, J. Appl. Crystallogr., 1999, 32, 837-838.
;
_computing_structure_refinement
;
      'SHELXS-2014 (Sheldrick, 2015)'
      Sheldrick, G. M. (2015). Acta Cryst. C71, 3--8.
;
_computing_structure_solution
;
      'SHELXS-2014 (Sheldrick, 2015)'
      Sheldrick, G. M. (2015). Acta Cryst. A71, 3--8.
;
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0628883
_diffrn_orient_matrix_UB_12      -0.0642349
_diffrn_orient_matrix_UB_13      0.0599697
_diffrn_orient_matrix_UB_21      0.0114892
_diffrn_orient_matrix_UB_22      -0.1695989
_diffrn_orient_matrix_UB_23      -0.0243224
_diffrn_orient_matrix_UB_31      0.1976633
_diffrn_orient_matrix_UB_32      0.0301188
_diffrn_orient_matrix_UB_33      -0.0091305
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7536
_diffrn_reflns_point_group_measured_fraction_max 0.784
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.391
_diffrn_reflns_theta_min         3.75
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       needle
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 1006 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         4662
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0470P)^2^+0.3935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1417
_reflns_Friedel_coverage         0.512
_reflns_Friedel_fraction_full    0.625
_reflns_Friedel_fraction_max     0.572
_reflns_number_gt                3600
_reflns_number_total             4662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ob02255d2.cif
_cod_data_source_block           8-mcmt93b2
_cod_depositor_comments
'Adding full bibliography for 7157265--7157270.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7157270
_shelx_estimated_absorpt_t_min   0.774
_shelx_estimated_absorpt_t_max   0.956
_shelx_res_checksum              94606