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_7022734
_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), 90.1 mg phen (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 brown residue
was washed with acetone and resolved in 80 ml methanol. Green crystals of
[ReO(phen)(rac-Glyc2,3H-21PH+1-kO2,3,P)] . MeOH formed within 14 days at 4 \%C.
;
_chemical_formula_moiety         'C15 H14 N2 O7 P Re, C H4 O'
_chemical_formula_sum            'C16 H18 N2 O8 P Re'
_chemical_formula_weight         583.504
_chemical_name_common            '[ReO(phen)(rac-Glyc2,3H-21PH-kO2,3,P)].MeOH'
_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_phen_Glyc1P_po139_Steinborn
_audit_creation_date             25-Oct-2011
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             '26-July-12 created by MS'
_cell_angle_alpha                90.000(4)
_cell_angle_beta                 91.399(3)
_cell_angle_gamma                90.000(4)
_cell_formula_units_Z            4
_cell_length_a                   10.2979(5)
_cell_length_b                   9.0749(5)
_cell_length_c                   19.4763(7)
_cell_measurement_reflns_used    2096
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.3071
_cell_measurement_theta_min      4.1782
_cell_volume                     1819.56(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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 15.9809
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
1 omega 34.00 100.00 1.0000 60.0000
omega____ theta____ kappa____ phi______ frames
- 21.2306 179.0000 90.0000 66
2 omega -10.00 95.00 1.0000 60.0000
omega____ theta____ kappa____ phi______ frames
- 21.2306 38.0000 150.0000 105
3 omega 30.00 66.00 1.0000 60.0000
omega____ theta____ kappa____ phi______ frames
- 21.2306 77.0000 -90.0000 36
;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0303430000
_diffrn_orient_matrix_UB_12      0.0665196000
_diffrn_orient_matrix_UB_13      0.0100451000
_diffrn_orient_matrix_UB_21      -0.0595476000
_diffrn_orient_matrix_UB_22      -0.0248087000
_diffrn_orient_matrix_UB_23      -0.0149993000
_diffrn_orient_matrix_UB_31      -0.0166953000
_diffrn_orient_matrix_UB_32      -0.0327121000
_diffrn_orient_matrix_UB_33      0.0316448000
_diffrn_radiation_collimation    '0.5 mm collimator'
_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  0.0837
_diffrn_reflns_av_sigmaI/netI    0.1187
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6341
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         4.18
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.816
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.13006(16)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.571
_refine_diff_density_min         -2.382
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3673
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0093P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                2717
_reflns_number_total             3673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32901a.txt
_cod_data_source_block           po139
_cod_original_cell_volume        1819.56(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7022734