Biologically Relevant Phosphoranes: Structural Characterization of Glucofuranose- and Xylofuranose-Based Phosphoranes1
Timosheva, Natalya V.; Chandrasekaran, A.; Holmes, Robert R.; Inorganic Chemistry 45 (2006) 3113–3123; doi:10.1021/ic052105e

data_4332063
_publ_section_title
;
 Biologically Relevant Phosphoranes:&#x00A0; Structural Characterization
 of Glucofuranose- and Xylofuranose-Based Phosphoranes1
;
_journal_issue                   7
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3113
_journal_page_last               3123
_journal_paper_doi               10.1021/ic052105e
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C45 H65 O9 P'
_chemical_formula_weight         780.94
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.8160(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.0122(2)
_cell_length_b                   11.9486(2)
_cell_length_c                   17.6226(3)
_cell_measurement_reflns_used    3863
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      4.08
_cell_volume                     2231.00(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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    0.0349
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7255
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         4.21
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.9302
_exptl_absorpt_correction_T_min  0.9101
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.85
_exptl_crystal_size_min          0.65
_refine_diff_density_max         0.108
_refine_diff_density_min         -0.142
_refine_diff_density_rms         0.024
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         7255
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0375P)^2^+0.3020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                6495
_reflns_number_total             7255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic052105esup4.cif
_cod_data_source_block           ntp32(Compound=4)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4332063