Oxidorhenium(V) complexes with L-histidine and pyranosides.
Grimminger, Philipp; Klüfers, Peter; Dalton transactions (Cambridge, England : 2003) 39 (2010) 715–719; doi:10.1039/b912603a

data_7024194
_publ_section_title
;
 Oxidorhenium(V) complexes with L-histidine and pyranosides.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              715
_journal_page_last               719
_journal_paper_doi               10.1039/b912603a
_journal_volume                  39
_journal_year                    2010
_chemical_absolute_configuration syn
_chemical_compound_source
;
0.833 g (1.0 mmol) of the Rhenium(V)-oxo-complex trans-ReOCl3(PPh3)2 were
stirred with 0.388 g (2.0 mmol) methyl-\a-D-mannopyranoside, 0.155 g (1.0 mmol)
L-histidine and 0.303 g (3.0 mmol) triethylamine in
250 ml methanol. After stirring for 2 hours at 50 \%C the yellow suspension
turned into a blue solution. Then the volume was reduced in vakuo to 30 ml.
A blue powder of (I) was filtered off and recrystallised in methanol.
;
_chemical_formula_moiety         'C13 H20 N3 O9 Re, 2(C H4 O)'
_chemical_formula_sum            'C15 H28 N3 O11 Re'
_chemical_formula_weight         612.60
_chemical_name_common            ReO(His)(MeaDManp)
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                Re_O_His_MeaDManp_jn213_grimminger
_audit_creation_date             30-Juni-05
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             12-FEB-07
_cell_angle_alpha                90.00
_cell_angle_beta                 114.2054(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.2622(4)
_cell_length_b                   9.0735(2)
_cell_length_c                   10.4724(2)
_cell_measurement_reflns_used    14780
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     2189.40(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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 Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0024377
_diffrn_orient_matrix_UB_12      -0.0815764
_diffrn_orient_matrix_UB_13      0.0615719
_diffrn_orient_matrix_UB_21      0.0423847
_diffrn_orient_matrix_UB_22      0.0108926
_diffrn_orient_matrix_UB_23      0.0601631
_diffrn_orient_matrix_UB_31      -0.0090113
_diffrn_orient_matrix_UB_32      0.0733015
_diffrn_orient_matrix_UB_33      0.0595824
_diffrn_radiation_collimation    0.35
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19131
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.28
_diffrn_source_current           75.00
_diffrn_source_power             4.125
_diffrn_source_type              'FR 591 generator'
_diffrn_source_voltage           55.00
_exptl_absorpt_coefficient_mu    5.610
_exptl_absorpt_correction_T_max  0.7705
_exptl_absorpt_correction_T_min  0.4851
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Crystal faces optimized with XShape, rev. 1.02, STOE (Darmstadt, Germany)
Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.542
_refine_diff_density_min         -1.782
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.041(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4484
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0172P)^2^+1.8116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                4106
_reflns_number_total             4484
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b912603a.txt
_cod_data_source_block           jn213
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7024194
_kl_diffrn_measurement_scan_angle phi/omega-scan
_kl_diffrn_measurement_scan_step_degree 2.0
_kl_diffrn_measurement_scan_time_per_degree 30
_kl_diffrn_measurement_detector_distance 35