Molybdenum Complexes with Sterically Demanding Cycloheptatrienyl Ligands
Tamm, Matthias; Bannenberg, Thomas; Dressel, Bernd; Fröhlich, Roland; Kunz, Doris; Organometallics 20 (2001) 900–; doi:10.1021/om000830l

data_4077232
_publ_section_title
;
 Molybdenum Complexes with Sterically Demanding Cycloheptatrienyl Ligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              900
_journal_paper_doi               10.1021/om000830l
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C19 H31 B F4'
_chemical_formula_weight         346.25
_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                 101.57(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.223(5)
_cell_length_b                   10.936(3)
_cell_length_c                   18.195(6)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      21.15
_cell_volume                     1992.8(13)
_computing_cell_refinement       'Express (Nonius B.V., 1994)'
_computing_data_collection       'Express (Nonius B.V., 1994)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_sigmaI/netI    0.1192
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3502
_diffrn_reflns_theta_full        64.99
_diffrn_reflns_theta_max         64.99
_diffrn_reflns_theta_min         4.61
_diffrn_standards_decay_%        10.7
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.9283
_exptl_absorpt_correction_T_min  0.8952
_exptl_absorpt_correction_type   'empirical via \y scan data'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    'refined as riding atoms'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0887P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1694
_reflns_number_gt                1701
_reflns_number_total             3390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000830l.cif
_cod_data_source_block           han1222
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4077232