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_7157266
_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 H48 O4'
_chemical_formula_weight         520.72
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
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_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
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_audit_creation_date             2019-08-22T12:47:19-00:00
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_audit_update_record
;
2019-09-11 deposited with the CCDC.	2019-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.982(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3526(7)
_cell_length_b                   7.2237(3)
_cell_length_c                   19.7666(12)
_cell_measurement_reflns_used    4338
_cell_measurement_temperature    130(2)
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_cell_measurement_theta_min      3.973
_cell_volume                     1565.91(16)
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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)
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        CrysAlisPro, Agilent Technologies,
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        (compiled Aug  2 2013,16:46:58)
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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)
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_computing_molecular_graphics
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          'Ortep-3 for Windows (Farrugia, 1997)'
      L. J. Farrugia, J. Appl. Crystallogr., 1997, 30, 565.
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_computing_publication_material
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        'WinGX publication routines (Farrugia, 1999)'				 
	L. J. Farrugia, J. Appl. Crystallogr., 1999, 32, 837-838.
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_computing_structure_refinement
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      '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
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_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1039053
_diffrn_orient_matrix_UB_12      0.0550539
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_diffrn_orient_matrix_UB_21      -0.089986
_diffrn_orient_matrix_UB_22      -0.0034428
_diffrn_orient_matrix_UB_23      0.0465784
_diffrn_orient_matrix_UB_31      0.0292435
_diffrn_orient_matrix_UB_32      -0.205791
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_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0693
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_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
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_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14649
_diffrn_reflns_point_group_measured_fraction_max 0.744
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.106
_diffrn_reflns_theta_min         4.031
_exptl_absorpt_coefficient_mu    0.55
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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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)
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    1.104
_exptl_crystal_description       plate
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_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.146
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.037
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;
 Flack x determined using 1013 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4727
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.007
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0528P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.4
_reflns_Friedel_fraction_full    0.504
_reflns_Friedel_fraction_max     0.464
_reflns_number_gt                4048
_reflns_number_total             4727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ob02255d2.cif
_cod_data_source_block           7-mcmt105c2_sq
_cod_depositor_comments
'Adding full bibliography for 7157265--7157270.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7157266
_shelx_estimated_absorpt_t_min   0.802
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              15321
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