Crystal structure and absolute configuration of (3a<i>R</i>,3'a<i>R</i>,7a<i>S</i>,7'a<i>S</i>)-2,2,2',2'-tetramethyl-3a,6,7,7a,3'a,6',7',7'a-octahydro-4,4'-bi[1,3-benzodioxolyl], obtained from a Pd-catalyzed homocoupling reaction
Macías, Mario A.; Pandolfi, Enrique; Schapiro, Valeria; Silveira, Gustavo P.; Vilela, Guilherme D.; Suescun, Leopoldo; Acta Crystallographica Section E 73 (2017) 81–84; doi:10.1107/S2056989016019927

data_2241992
_publ_section_title
;
 Crystal structure and absolute configuration of
 (3a<i>R</i>,3'a<i>R</i>,7a<i>S</i>,7'a<i>S</i>)-2,2,2',2'-tetramethyl-3a,6,7,7a,3'a,6',7',7'a-octahydro-4,4'-bi[1,3-benzodioxolyl],
 obtained from a Pd-catalyzed homocoupling reaction
;
_journal_coeditor_code           RZ5201
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              81
_journal_page_last               84
_journal_paper_doi               10.1107/S2056989016019927
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C18 H26 O4'
_chemical_formula_moiety         'C18 H26 O4'
_chemical_formula_sum            'C18 H26 O4'
_chemical_formula_weight         306.39
_chemical_name_systematic
(3a<i>R</i>,3'a<i>R</i>,7a<i>S</i>,7'a<i>S</i>)-2,2,2',2'-Tetramethyl-3a,6,7,7a,3'a,6',7',7'a-octahydro-4,4'-bi[1,3-benzodioxolyl]
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 95.216(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.2927(7)
_cell_length_b                   17.9903(19)
_cell_length_c                   7.2991(8)
_cell_measurement_reflns_used    9685
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      72.3851
_cell_measurement_theta_min      4.9165
_cell_volume                     822.89(16)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008, 2015)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008, 2015)
;
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            27011
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.378
_diffrn_reflns_theta_min         4.916
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.133
_refine_diff_density_min         -0.101
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1475 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_coef       0.0184(15)
_refine_ls_extinction_expression
;
<i>F</i>~c~^*^ =
<i>k</i><i>F</i>~c~[1+0.001<i>x</i><i>F</i>~c~^2^\l^3^/sin(2\q)]^-1/4^
;
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3232
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0389P)^2^+0.0652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                3135
_reflns_number_total             3232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rz5201sup1.cif
_cod_data_source_block           I
_cod_database_code               2241992
_cod_database_fobs_code          2241992
_shelx_estimated_absorpt_t_min   0.769
_shelx_estimated_absorpt_t_max   0.819
_shelx_hkl_checksum              35563
_shelx_res_checksum              64824
_shelxl_version_number           2.014