Trigonal Prismatic Structure of Tris(butadiene)molybdenum and Related Complexes Revisited: Diolefin or Metallacyclopentene Coordination?
Kaupp, Martin; Kopf, Thomas; Murso, Alexander; Stalke, Dietmar; Strohmann, Carsten; Hanks, John R.; Cloke, F. Geoffrey N.; Hitchcock, Peter B.; Organometallics 21 (2002) 5021–; doi:10.1021/om020525v

data_4077065
_publ_contact_author             'Prof. Dr. Dietmar Stalke'
_publ_section_title
;
 Trigonal Prismatic Structure of Tris(butadiene)molybdenum and Related
 Complexes Revisited:&#x00A0; Diolefin or Metallacyclopentene
 Coordination?
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5021
_journal_paper_doi               10.1021/om020525v
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C12 H18 Mo'
_chemical_formula_weight         258.20
_chemical_name_common            '[Mo(butadiene)3]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   7.2142(10)
_cell_length_b                   7.2142(10)
_cell_length_c                   11.802(2)
_cell_measurement_reflns_used    5108
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      3.705
_cell_volume                     531.94(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'XP in SHELXTL-97'
_computing_publication_material  'XP in SHELXTL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       CCD
_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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3263
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         4.75
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         445
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0190
_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^)+(0.0204P)^2^+0.2754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0436
_refine_ls_wR_factor_ref         0.0444
_reflns_number_gt                420
_reflns_number_total             451
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            om020525v.cif
_cod_data_source_block           compound_1
_cod_original_cell_volume        531.94(15)
_cod_original_sg_symbol_H-M      P6(3)/m
_cod_database_code               4077065