Structural and Spectroscopic Characterization of 17- and 18-Electron Piano-Stool Complexes of Chromium. Thermochemical Analyses of Weak Cr-H Bonds
Edwin F. van der Eide; Monte L. Helm; Eric D. Walter; R. Morris Bullock; Inorganic Chemistry 52 (2013) 1591–1603; doi:10.1021/ic302460y

data_4333748
_publ_contact_author_address
;
Pacific Northwest National Laboratory
PO Box 999
Richland, WA 99352
USA
;
_publ_contact_author_name        'Monte L. Helm'
_publ_section_title
;
 Structural and Spectroscopic Characterization of 17- and 18-Electron
 Piano-Stool Complexes of Chromium. Thermochemical Analyses of Weak Cr-H
 Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1591
_journal_page_last               1603
_journal_paper_doi               10.1021/ic302460y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C52 H60 Cr4 K4 N8 O9, 2(C4 H8 O)'
_chemical_formula_sum            'C60 H76 Cr4 K4 N8 O11'
_chemical_formula_weight         1449.69
_chemical_name_common            K[CpCr(CO)2(IMe)]
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.219(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.5173(2)
_cell_length_b                   25.0725(6)
_cell_length_c                   17.4342(4)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.79
_cell_measurement_theta_min      2.50
_cell_volume                     3252.20(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            74260
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  0.9352
_exptl_absorpt_correction_T_min  0.8372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.237
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 7135 Friedel pairs'
_refine_ls_abs_structure_Flack   0.004(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         15106
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+1.2934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                13324
_reflns_number_total             15106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302460y_si_002_3.cif
_cod_data_source_block           helm069_0m
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4333748