A structural study of [CpM(CO)3H] (M = Cr, Mo and W) by single-crystal X-ray diffraction and DFT calculations: sterically crowded yet surprisingly flexible molecules
Burchell, Richard P. L.; Sirsch, Peter; Decken, Andreas; McGrady, G. Sean; Dalton Transactions  (2009) 5851–5857; doi:10.1039/b902612f

data_7001751
_publ_section_title
;
 A structural study of [CpM(CO)3H] (M = Cr, Mo and W) by single-crystal
 X-ray diffraction and DFT calculations: sterically crowded yet
 surprisingly flexible molecules
;
_journal_issue                   30
_journal_name_full               'Dalton Transactions'
_journal_page_first              5851
_journal_page_last               5857
_journal_paper_doi               10.1039/b902612f
_journal_year                    2009
_chemical_formula_moiety         'C8 H6 Mo O3'
_chemical_formula_sum            'C8 H6 Mo O3'
_chemical_formula_weight         246.07
_chemical_name_systematic
;
Tricarbonylcyclopentadienylhydridomolybdenum(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.943(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1449(14)
_cell_length_b                   7.5856(10)
_cell_length_c                   11.617(2)
_cell_measurement_reflns_used    4504
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.69
_cell_volume                     867.6(2)
_computing_cell_refinement
;
Bruker (1999). SMART, version 5.054, Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_data_collection
;
Bruker (1999). SMART, version 5.054, Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_data_reduction
;
Bruker (2001). SAINT, version 7.23a, Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_molecular_graphics
;
Farrugia, L. J. (1997) ORTEP-3. J Appl. Crystallogr. 30, 565.
;
_computing_publication_material
;
Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_structure_refinement
;
Sheldrick, G. M. (1997). SHELXL97. University of
Gottingen, Germany.
;
_computing_structure_solution
;
Sheldrick, G. M. (1997). SHELXS97. University of
Gottingen, Germany.
;
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker AXS SMART1000/P4'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5834
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.07
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.472
_exptl_absorpt_correction_T_max  0.742056
_exptl_absorpt_correction_T_min  0.57869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.344
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0224
_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^)+(0.0401P)^2^+0.2150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0632
_reflns_number_gt                1796
_reflns_number_total             1942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            b902612f.txt
_cod_data_source_block           sg080467
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7001751