A retro diels-alder route to diphosphorus chemistry: molecular precursor synthesis, kinetics of p2 transfer to 1,3-dienes, and detection of p2 by molecular beam mass spectrometry.
Velian, Alexandra; Nava, Matthew; Temprado, Manuel; Zhou, Yan; Field, Robert W.; Cummins, Christopher C.; Journal of the American Chemical Society 136 (2014) 13586–13589; doi:10.1021/ja507922x

data_4122640
_publ_section_title
;
 A retro diels-alder route to diphosphorus chemistry: molecular precursor
 synthesis, kinetics of p2 transfer to 1,3-dienes, and detection of p2 by
 molecular beam mass spectrometry.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13586
_journal_page_last               13589
_journal_paper_doi               10.1021/ja507922x
_journal_volume                  136
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C14 H10 Cl P'
_chemical_formula_weight         244.64
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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
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_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.656(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
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_cell_length_b                   6.1042(7)
_cell_length_c                   11.6311(13)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.59
_cell_measurement_theta_min      2.59
_cell_volume                     559.05(11)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
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_diffrn_reflns_limit_h_max       12
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_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14712
_diffrn_reflns_theta_full        31.59
_diffrn_reflns_theta_max         31.59
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.449
_exptl_absorpt_correction_T_max  0.9736
_exptl_absorpt_correction_T_min  0.8269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             252
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         3721
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+0.1406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0773
_reflns_number_gt                3598
_reflns_number_total             3721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ClPA.cif
_cod_data_source_block           final
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4122640--4122642.cif.
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_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4122640