Redox routes to arenechromium complexes of two-, three- and four-electron alkynes; structure and bonding in paramagnetic [Cr(CO)L(η-RCCR)(η-arene)]+
Christopher J. Adams; Ian M. Bartlett; Neil G. Connelly; David J. Harding; Owen D. Hayward; Antonio J. Martín; A. Guy Orpen; Michael J. Quayle; Philip H. Rieger; J. Chem. Soc., Dalton Trans.  (2002) 4281–4288; doi:10.1039/b206177p

data_7011963
_publ_section_title
;
 Redox routes to arenechromium complexes of two-, three- and
 four-electron alkynes; structure and bonding in paramagnetic
 [Cr(CO)L(\h-RCCR)(\h-arene)]+
;
_journal_issue                   22
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4281
_journal_page_last               4288
_journal_paper_doi               10.1039/b206177p
_journal_year                    2002
_chemical_formula_sum            'C38 H41 Cr F6 N O3 P'
_chemical_formula_weight         756.69
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.917(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1760(17)
_cell_length_b                   22.284(5)
_cell_length_c                   14.739(2)
_cell_measurement_reflns_used    254
_cell_measurement_temperature    173(2)
_cell_volume                     3547.0(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans with narrow frames'
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18328
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  0.9785
_exptl_absorpt_correction_T_min  0.9785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_crystal_colour            red-black
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         6232
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0345P)^2^+8.3537P] where 
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1405
_reflns_number_gt                4786
_reflns_number_total             6232
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206177p.txt
_cod_data_source_block           7plus
_cod_original_cell_volume        3547.1(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7011963