Umpolung catalyzed by organophosphines: efficient β,β-dimerization of vinylphosphonates affording linear dimers
Wang, Xiang-Bo; Saga, Yuta; Shen, Ruwei; Fujino, Hiroyoshi; Goto, Midori; Han, Li-Biao; RSC Advances 2 (2012) 5935–; doi:10.1039/c2ra20704d

data_7238672
_publ_section_title
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 Umpolung catalyzed by organophosphines: efficient \b,\b-dimerization of
 vinylphosphonates affording linear dimers
;
_journal_issue                   14
_journal_name_full               'RSC Advances'
_journal_page_first              5935
_journal_paper_doi               10.1039/c2ra20704d
_journal_volume                  2
_journal_year                    2012
_chemical_formula_moiety         'C7 H18 O3 P", H2 O'
_chemical_formula_sum            'C7 H20 O4 P2'
_chemical_formula_weight         230.17
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.122(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   8.8559(11)
_cell_length_b                   23.483(3)
_cell_length_c                   17.042(2)
_cell_measurement_reflns_used    7272
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.39
_cell_volume                     3544.1(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating unit'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0253
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_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19135
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.9881
_exptl_absorpt_correction_T_min  0.9245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.818
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_refine_ls_extinction_method     none
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_refine_ls_number_parameters     386
_refine_ls_number_reflns         7493
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+2.6397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                6376
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra20704d.txt
_cod_data_source_block           hanwang1
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_atom_sites_solution_hydrogens' value 'geom and difmap'
was changed to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_cell_volume        3544.0(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7238672