Mixed sugar-core-phosphate chelation of D-fructose 1,6-bisphosphate with the Re(V)O(tmen) metal fragment.
Steinborn, Martin; Suhanji, Mihael; Klüfers, Peter; Dalton transactions (Cambridge, England : 2003) 42 (2013) 5749–5754; doi:10.1039/c3dt32901a

data_7022733
_publ_section_title
;
 Mixed sugar-core-phosphate chelation of D-fructose 1,6-bisphosphate with
 the Re(V)O(tmen) metal fragment.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5749
_journal_page_last               5754
_journal_paper_doi               10.1039/c3dt32901a
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration rm
_chemical_compound_source
;
418 mg trans-[ReOCl3(PPh3)2] (0.5 mmol), 0.0750 ml tmen (0.5 mmol), 108 mg
Na2-rac-Glyc1PxxH2O (0.5 mmol) and 0.1386 ml NEt3 (1.0 mmol) in 250 ml methanol
were stirred at RT for 48 hours. After removing the solvent the blue residue
was solved in 40 ml acetone. After removing colourless crystals by filtration
blue crystals of [ReO(tmen)(rac-Glyc1P2,3H-2PH+1-kO2,3,P)] . 2 H2O formed
within 5 hours at RT.
;
_chemical_formula_moiety         'C9 H22 N2 O7 P Re, 2(H2 O)'
_chemical_formula_sum            'C9 H26 N2 O9 P Re'
_chemical_formula_weight         523.492
_chemical_name_common            '[ReO(tmen)(rac-Glyc1P2,3H-2PH-kO2,3,P)].2H2O'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                Re_tmen_Glyc1P_pn362_Steinborn
_audit_creation_date
;
03-Nov-11
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record
;
26-July-12 created by MS
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 111.0465(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.1114(5)
_cell_length_b                   7.5592(5)
_cell_length_c                   16.5961(5)
_cell_measurement_reflns_used    6860
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     1652.22(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0383383
_diffrn_orient_matrix_UB_12      0.1140995
_diffrn_orient_matrix_UB_13      -0.0096616
_diffrn_orient_matrix_UB_21      0.0463596
_diffrn_orient_matrix_UB_22      0.0508877
_diffrn_orient_matrix_UB_23      -0.0275570
_diffrn_orient_matrix_UB_31      -0.0463286
_diffrn_orient_matrix_UB_32      -0.0434990
_diffrn_orient_matrix_UB_33      -0.0575806
_diffrn_radiation_collimation    0.20
_diffrn_radiation_monochromator  'MONTEL, graded multilayered X-ray optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27719
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         3.15
_diffrn_source_current           55.00
_diffrn_source_power             3.025
_diffrn_source_type              'FR 591 generator'
_diffrn_source_voltage           55.00
_exptl_absorpt_coefficient_mu    7.496
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G.M. SADABS. Version 2. Multi-Scan Absorption Correction Program.
University of G\"ottingen, Germany, 2001.
\m \\times r = xxx, Tmin/Tmax = yyy
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.10454(17)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.834
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3808
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0029P)^2^+6.6091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0549
_reflns_number_gt                3372
_reflns_number_total             3808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32901a.txt
_cod_data_source_block           pn362
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7022733