Diels-Alder reactions of 1-phosphabutadienes: a highly selective route to P[double bond, length as m-dash]C-substituted phosphacyclohexenes.
Ohtsuki, Kazuaki; Walsgrove, Henry T. G.; Hayashi, Yoshihiro; Kawauchi, Susumu; Patrick, Brian O.; Gates, Derek P.; Ito, Shigekazu; Chemical communications (Cambridge, England) 56 (2020) 774–777; doi:10.1039/c9cc08997g

data_7125799
_publ_section_title
;
 Diels-Alder reactions of 1-phosphabutadienes: a highly selective route to
 P[double bond, length as m-dash]C-substituted phosphacyclohexenes.
;
_journal_issue                   5
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              774
_journal_page_last               777
_journal_paper_doi               10.1039/c9cc08997g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_sum            'C42 H64 Br2 P2'
_chemical_formula_weight         790.69
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-09-09 deposited with the CCDC.	2019-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_measurement_reflns_used    279
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.478
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_cell_volume                     4127.3(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  RAXIS-Rapid
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.1132
_diffrn_reflns_Laue_measured_fraction_full 0.888
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       19
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_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_point_group_measured_fraction_full 0.888
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_exptl_absorpt_coefficient_mu    2.068
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_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
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_exptl_crystal_description       platelet
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.110
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_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.394
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_refine_ls_extinction_method     none
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1904
_refine_ls_wR_factor_ref         0.2323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4993
_reflns_number_total             8464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08997g2.cif
_cod_data_source_block           Ohtsuki
_cod_depositor_comments
'Adding full bibliography for 7125799--7125801.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7125799
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.804
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_shelx_res_checksum              88696