<i>cis</i>-Dichlorido[2,3-dimethyl-3-(4,4,5,5-tetramethyl-1,3,2λ^5^-dioxaphospholan-2-yloxy)butan-2-olato-κ^2^<i>O</i>,<i>P</i>]oxido(triphenylphosphane-κ<i>P</i>)rhenium(V)
Skarżyńska, Anna; Siczek, Miłosz; Gniewek, Andrzej; Acta Crystallographica Section E 68 (2012) m605–m606; doi:10.1107/S1600536812015565

data_2234810
_publ_section_title
;
 <i>cis</i>-Dichlorido[2,3-dimethyl-3-(4,4,5,5-tetramethyl-1,3,2\l^5^-dioxaphospholan-2-yloxy)butan-2-olato-\k^2^<i>O</i>,<i>P</i>]oxido(triphenylphosphane-\k<i>P</i>)rhenium(V)
;
_journal_coeditor_code           SU2403
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m605
_journal_page_last               m606
_journal_paper_doi               10.1107/S1600536812015565
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Re (C12 H24 O4 P) Cl2 O (C18 H15 P)]'
_chemical_formula_moiety         'C30 H39 Cl2 O5 P2 Re'
_chemical_formula_sum            'C30 H39 Cl2 O5 P2 Re'
_chemical_formula_weight         798.65
_chemical_name_systematic
;
<i>cis</i>-Dichlorido[2,3-dimethyl-3-(4,4,5,5-tetramethyl-1,3,2\l^5^-
dioxaphospholan-2-yloxy)butan-2-olato-
\k^2^<i>O</i>,<i>P</i>]oxido(triphenylphosphane-\k<i>P</i>)rhenium(V)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.963(3)
_cell_length_b                   16.328(4)
_cell_length_c                   17.797(5)
_cell_measurement_reflns_used    8908
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      4.75
_cell_volume                     3185.7(15)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2010)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur PX diffractometer with a CCD detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15943
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         4.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.119
_exptl_absorpt_correction_T_max  0.808
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2010)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.214
_refine_diff_density_min         -1.086
_refine_ls_abs_structure_details 'Flack (1983), 3463 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.015(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         8614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0111P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0438
_refine_ls_wR_factor_ref         0.0455
_reflns_number_gt                6813
_reflns_number_total             8614
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2403.cif
_cod_data_source_block           I
_cod_database_code               2234810
_cod_database_fobs_code          2234810