High Pressure promoted Dearomatization of Nitroarenes by [4+2] Cycloadditions with Silyloxydienes
Rkein, Batoul; Coffinier, Romain; Powderly, Marian; Manneveau, Maxime; Sanselme, Morgane; Durandetti, Muriel; Sebban, Muriel; Hamdoun, Ghanem; Oulyadi, Hassan; Harrowven, David; Legros, Julien; Chataigner, Isabelle; Chemical Communications  (2022) –; doi:10.1039/D2CC04778K

data_7130768
_publ_section_title
;
 High Pressure promoted Dearomatization of Nitroarenes by [4+2]
 Cycloadditions with Silyloxydienes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04778K
_journal_year                    2022
_chemical_formula_moiety         'P3 Sr3 Zn'
_chemical_formula_sum            'P3 Sr3 Zn'
_chemical_formula_weight         421.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_primary     dual
_audit_block_doi                 10.25505/fiz.icsd.cc2b6wt8
_audit_creation_date             2020-09-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2022-02-11 deposited with the CCDC.	2022-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.677(3)
_cell_length_b                   9.403(2)
_cell_length_c                   12.794(3)
_cell_measurement_reflns_used    3603
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      29.27
_cell_measurement_theta_min      2.69
_cell_volume                     1404.8(6)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17785
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.632
_diffrn_reflns_theta_min         2.361
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    26.588
_exptl_absorpt_correction_T_max  0.2644
_exptl_absorpt_correction_T_min  0.1404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1125 before and 0.0465 after correction.
The Ratio of minimum to maximum transmission is 0.5310.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.982
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.099
_refine_diff_density_max         1.452
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       0.00056(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         2089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+1.6160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0532
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1708
_reflns_number_total             2089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04778k2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1404.8(5)
_cod_database_code               7130768
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.178
_shelx_estimated_absorpt_t_min   0.124
_olex2_refinement_description
;
;
_shelx_res_checksum              85739
_shelx_hkl_checksum              51712
_olex2_submission_special_instructions 'No special instructions were received'