Synthesis and Characterization of Organometallic Ionic Liquids and a Heterometallic Carbene Complex Containing the Chromium Tricarbonyl Fragment
Moret, Marc-Etienne; Chaplin, Adrian B.; Lawrence, Adrien K.; Scopelliti, Rosario; Dyson, Paul J.; Organometallics 24 (2005) 4039–; doi:10.1021/om050283+

data_4083953
_publ_section_title
;
 Synthesis and Characterization of Organometallic Ionic Liquids and a
 Heterometallic Carbene Complex Containing the Chromium Tricarbonyl
 Fragment
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4039
_journal_paper_doi               10.1021/om050283+
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C21 H24 Cr N O6 S, Br'
_chemical_formula_sum            'C21 H24 Br Cr N O6 S'
_chemical_formula_weight         550.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.63(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.232(5)
_cell_length_b                   11.169(4)
_cell_length_c                   12.166(2)
_cell_measurement_reflns_used    1886
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      18.9448
_cell_measurement_theta_min      1.25625
_cell_volume                     2293.4(11)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'marresearch, mar345'
_computing_data_reduction        'Oxford Diffraction CrysAlis RED'
_computing_molecular_graphics    'Cystal Impact DIAMOND'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'MAR345 IPDS'
_diffrn_measurement_method
'60 images with deltaphi = 3 deg. and exp. time = 180 sec.'
_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  0.1014
_diffrn_reflns_av_sigmaI/netI    0.1177
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14142
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    2.369
_exptl_absorpt_correction_T_max  0.3098
_exptl_absorpt_correction_T_min  0.2718
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
; 
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0633
_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^)+(0.0921P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1854
_reflns_number_gt                2021
_reflns_number_total             4050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050283%2Bsi20050527_114243.cif
_cod_data_source_block           pd191
_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/retrospective/ACS/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_cell_volume        2293.2(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4083953