Ring Expansion versusexo−endoIsomerization in (2-Pyridyl)methylenecyclobutane Coordinated to Hydrido(trispyrazolyl)borate- and Cyclopentadienyl-Osmium Complexes
Castro-Rodrigo, Ruth; Esteruelas, Miguel A.; López, Ana M.; López, Fernando; Mascareñas, José L.; Mozo, Silvia; Oñate, Enrique; Saya, Lucía; Organometallics 29 (2010) 2372–; doi:10.1021/om100243w

data_4066000
_publ_section_title
;
 Ring Expansion versusexo&#x2212;endoIsomerization in
 (2-Pyridyl)methylenecyclobutane Coordinated to
 Hydrido(trispyrazolyl)borate- and Cyclopentadienyl-Osmium Complexes
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2372
_journal_paper_doi               10.1021/om100243w
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C28.5 H43 B Cl F6 N7 Os P2'
_chemical_formula_weight         896.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.9919(17)
_cell_length_b                   31.304(3)
_cell_length_c                   14.8308(17)
_cell_measurement_reflns_used    4173
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2.3
_cell_volume                     6960.2(13)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.1160
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            73782
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.85
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.897
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             3560
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.375
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         8780
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+27.4355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                5685
_reflns_number_total             8780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100243w_si_001.cif
_cod_data_source_block           mae393as
_cod_original_cell_volume        6960.1(14)
_cod_original_sg_symbol_H-M      Pccn
_cod_original_formula_sum        'C28.50 H43 B Cl F6 N7 Os P2'
_cod_database_code               4066000