Substituent Effects on the Electrochemical, Spectroscopic, and Structural Properties of Fischer Mono- and Biscarbene Complexes of Chromium(0)
Belinda van der Westhuizen; Pieter J. Swarts; Louise M. van Jaarsveld; David C. Liles; Uwe Siegert; Jannie C. Swarts; Israel Fernández; Daniela I. Bezuidenhout; Inorganic Chemistry 52 (2013) 6674–6684; doi:10.1021/ic4007422

data_4335121
_publ_section_title
;
 Substituent Effects on the Electrochemical, Spectroscopic, and Structural
 Properties of Fischer Mono- and Biscarbene Complexes of Chromium(0)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6674
_journal_page_last               6684
_journal_paper_doi               10.1021/ic4007422
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C20 H12 Cr2 O13'
_chemical_formula_sum            'C20 H12 Cr2 O13'
_chemical_formula_weight         564.30
_chemical_name_systematic
;
 \m-Furan-2,5-diylbis(ethoxycarbene)-bis[pentacarbonylchromium(0)]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     intrinsic-phasing
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                89.575(2)
_cell_angle_beta                 88.030(2)
_cell_angle_gamma                87.423(2)
_cell_formula_units_Z            4
_cell_length_a                   6.2838(5)
_cell_length_b                   12.6526(9)
_cell_length_c                   29.1888(19)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      49.568
_cell_measurement_theta_min      5.271
_cell_volume                     2316.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
; <i>ORTEP-3 for Windows</i> (Farrugia, 1997), <i>POV-RAY</i> (Cason, 2004),
 <i>Mercury</i> (Macrae <i>et al</i>., 2008)
;
_computing_publication_material
' <i>SHELXL-2012</i>, <i>PLATON</i> (Spek, 2009)'
_computing_structure_refinement
' Bruker SHELXTL, SHELXL-2012 (Sheldrick, 2012)''
_computing_structure_solution    'Bruker SHELXTS (Sheldrick, 2008, 2012)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker kappa Photon CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar multi-layer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            92144
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.040
_diffrn_reflns_theta_max         25.040
_diffrn_reflns_theta_min         2.138
_diffrn_source                   ' I\mS  micro focus'
_exptl_absorpt_coefficient_mu    1.005
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       needle
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         8131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+2.2628P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                6451
_reflns_number_total             8131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic4007422_si_001.cif
_cod_data_source_block           mo_BvdW1045A_0m_a
_cod_database_code               4335121
_shelxl_version_number           2012-9
_shelx_res_checksum              58912