Interaction of tertiary phosphines with lignin-type, alpha,beta-unsaturated aldehydes in water.
Moiseev, Dmitry V.; Patrick, Brian O.; James, Brian R.; Hu, Thomas Q.; Inorganic chemistry 46 (2007) 9389–9399; doi:10.1021/ic7007478

data_4333340
_publ_section_title
;
 Interaction of tertiary phosphines with lignin-type,
 alpha,beta-unsaturated aldehydes in water.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9389
_journal_page_last               9399
_journal_paper_doi               10.1021/ic7007478
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C30 H50 Cl2 O9 P2'
_chemical_formula_weight         687.54
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.084(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1860(10)
_cell_length_b                   31.887(3)
_cell_length_c                   11.3140(10)
_cell_measurement_reflns_used    4765
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.31
_cell_measurement_theta_min      2.55
_cell_volume                     3593.4(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25539
_diffrn_reflns_theta_full        25.27
_diffrn_reflns_theta_max         25.27
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         6455
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+2.7123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                4705
_reflns_number_total             6455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7007478sup2.cif
_cod_data_source_block           bj450
_cod_depositor_comments
'Adding full bibliography for 4333339--4333340.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4333340