Biologically relevant phosphoranes: synthesis and structural characterization of glucofuranose-derived phosphoranes with penta- and hexacoordination at phosphorus.
Timosheva, Natalya V.; Chandrasekaran, A.; Holmes, Robert R.; Inorganic chemistry 45 (2006) 10836–10848; doi:10.1021/ic061596f

data_4350607
_publ_section_title
;
 Biologically relevant phosphoranes: synthesis and structural
 characterization of glucofuranose-derived phosphoranes with penta- and
 hexacoordination at phosphorus.
;
_journal_issue                   26
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10836
_journal_page_last               10848
_journal_paper_doi               10.1021/ic061596f
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C31 H41 O8 P S'
_chemical_formula_weight         604.67
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 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                 112.281(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.7011(18)
_cell_length_b                   9.3468(10)
_cell_length_c                   15.544(2)
_cell_measurement_reflns_used    1809
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.98
_cell_measurement_theta_min      4.08
_cell_volume                     1842.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Nonius KappaCCD 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1259
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3345
_diffrn_reflns_theta_full        20.41
_diffrn_reflns_theta_max         20.41
_diffrn_reflns_theta_min         4.25
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.9957
_exptl_absorpt_correction_T_min  0.9038
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         3345
_refine_ls_number_restraints     475
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1728
_refine_ls_R_factor_gt           0.1443
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+20.9361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2897
_refine_ls_wR_factor_ref         0.3077
_reflns_number_gt                2666
_reflns_number_total             3345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061596fsi20060918_073910.cif
_cod_data_source_block           ntp40a_(compound_=_5)
_cod_depositor_comments
;
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/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4350607