Reaction of Spiro[2.4]hepta-4,6-diene with Molybdenum(II) Indenyl Compounds: Effects of Substitution in the Indenyl Ligand
Honzíček, Jan; Romão, Carlos C.; Calhorda, Maria J.; Mukhopadhyay, Abhik; Vinklárek, Jaromír; Padělková, Zdeňka; Organometallics 30 (2011) 717–; doi:10.1021/om100840r

data_4063689
_publ_section_title
;
 Reaction of Spiro[2.4]hepta-4,6-diene with Molybdenum(II) Indenyl
 Compounds: Effects of Substitution in the Indenyl Ligand
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              717
_journal_paper_doi               10.1021/om100840r
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C29 H23 Mo O, B F4'
_chemical_formula_sum            'C29 H23 B F4 Mo O'
_chemical_formula_weight         570.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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
_cell_angle_beta                 110.860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6430(8)
_cell_length_b                   11.9781(6)
_cell_length_c                   22.1769(17)
_cell_measurement_reflns_used    15392
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      1
_cell_volume                     2393.6(3)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_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  0.0714
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15334
_diffrn_reflns_theta_full        26.60
_diffrn_reflns_theta_max         26.60
_diffrn_reflns_theta_min         1.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0390P)^2^+9.6409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                3474
_reflns_number_total             4981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100840r_si_001.cif
_cod_data_source_block           19
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4063689