Crystal structure of <i>fac</i>-aquatricarbonyl[(<i>S</i>)-valinato-κ^2^<i>N</i>,<i>O</i>]rhenium(I)
Piletska, Kseniia O.; Domasevitch, Kostiantyn V.; Shtemenko, Alexander V.; Acta Crystallographica Section E 72 (2016) 590–592; doi:10.1107/S2056989016005235

data_2241621
_publ_section_title
;
 Crystal structure of
 <i>fac</i>-aquatricarbonyl[(<i>S</i>)-valinato-\k^2^<i>N</i>,<i>O</i>]rhenium(I)
;
_journal_coeditor_code           WM5283
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              590
_journal_page_last               592
_journal_paper_doi               10.1107/S2056989016005235
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Re (C5 H10 N O2) (C O)3 (H2 O)]'
_chemical_formula_moiety         'C8 H12 N O6 Re'
_chemical_formula_sum            'C8 H12 N O6 Re'
_chemical_formula_weight         404.39
_chemical_name_systematic
;
<i>fac</i>-Aquatricarbonyl[(<i>S</i>)-valinato-\
\k^2^<i>N</i>,<i>O</i>]rhenium(I)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1229(5)
_cell_length_b                   7.2913(7)
_cell_length_c                   22.6098(18)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.94
_cell_volume                     1174.24(17)
_computing_cell_refinement
;
IPDS Software (Stoe, 2000)
;
_computing_data_collection
;
IPDS Software (Stoe, 2000)
;
_computing_data_reduction
;
IPDS Software (Stoe, 2000)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL-2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe Imaging plate diffraction system'
_diffrn_measurement_method       '\f oscillation scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            10442
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.981
_diffrn_reflns_theta_min         2.935
_exptl_absorpt_coefficient_mu    10.360
_exptl_absorpt_correction_T_max  0.3695
_exptl_absorpt_correction_T_min  0.2880
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(<i>X-SHAPE</i> and <i>X-RED</i>; Stoe, 2001)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.287
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.683
_refine_diff_density_min         -0.906
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 990 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013).
;
_refine_ls_abs_structure_Flack   -0.018(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0254P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0473
_reflns_number_gt                2546
_reflns_number_total             2809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5283sup1.cif
_cod_data_source_block           I
_cod_database_code               2241621
_shelx_estimated_absorpt_t_min   0.288
_shelx_estimated_absorpt_t_max   0.369
_shelx_hkl_checksum              6606
_shelx_res_checksum              20551
_cod_database_fobs_code 2241621