Synthesis and characterisation of chelated cationic ReI(CO)3bis(NHC)(WCA) complexes.
Hock, Sebastian J.; Schaper, Lars-Arne; Pöthig, Alexander; Drees, Markus; Herdtweck, Eberhardt; Hiltner, Oliver; Herrmann, Wolfgang A.; Kühn, Fritz E; Dalton transactions (Cambridge, England : 2003) 43 (2014) 2259–2271; doi:10.1039/c3dt52605d

data_7028820
_publ_section_title
;
 Synthesis and characterisation of chelated cationic ReI(CO)3bis(NHC)(WCA)
 complexes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2259
_journal_page_last               2271
_journal_paper_doi               10.1039/c3dt52605d
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C33 H37 N5 O3 Re, F6 P'
_chemical_formula_sum            'C33 H37 F6 N5 O3 P Re'
_chemical_formula_weight         882.86
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 101.758(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.2454(9)
_cell_length_b                   8.9066(2)
_cell_length_c                   27.3469(8)
_cell_measurement_reflns_used    9242
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.4486
_cell_measurement_theta_min      2.4506
_cell_volume                     7927.6(4)
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed-tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            48269
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.46
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    3.170
_exptl_absorpt_correction_T_max  0.364
_exptl_absorpt_correction_T_min  0.275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_platon_squeeze_details
;
The unit cell contains 8 diethylether molecules which have been treated as a 
diffuse contribution to the overall scattering without specific atom positions 
by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.884
_refine_diff_density_min         -1.872
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         7320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.289
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.003
_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^+93.1056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                6969
_reflns_number_total             7320
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3dt52605d.txt
_cod_data_source_block           Compound_3c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7028820