Synthesis, Structure, and Ligand Exchange Reactions of Tetramethyleneethane Complexes of Cobalt
Aguirre-Etcheverry, Paulina; Ashley, Andrew E.; Balázs, Gábor; Green, Jennifer C.; Cowley, Andrew R.; Thompson, Amber L.; O’Hare, Dermot; Organometallics 29 (2010) 5847–; doi:10.1021/om100611p

data_4066748
_publ_section_title
;
 Synthesis, Structure, and Ligand Exchange Reactions of
 Tetramethyleneethane Complexes of Cobalt
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5847
_journal_paper_doi               10.1021/om100611p
_journal_volume                  29
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_compound_source        'oxidation of TME cobalt carbonyl'
_chemical_formula_moiety         'C11 H8 B1 Co2 F4 O5'
_chemical_formula_sum            'C11 H8 B Co2 F4 O5'
_chemical_formula_weight         424.85
_chemical_name_common            'TME Co Carbonyl oxidised'
_chemical_name_systematic        '[Co(CO)3]TME[Co(CO)2]BF4'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-01-04
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4109(2)
_cell_length_b                   12.9909(3)
_cell_length_c                   15.0675(4)
_cell_measurement_reflns_used    1911
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1450.61(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22999
_diffrn_reflns_theta_full        27.430
_diffrn_reflns_theta_max         27.430
_diffrn_reflns_theta_min         5.131
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.351
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            translucent_dark_brown
_exptl_crystal_density_diffrn    1.945
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             836
_exptl_crystal_recrystallization_method hexane
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.38
_refine_ls_abs_structure_details 'Flack (1983), 1421 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.259(14)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0873
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3034
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.000465
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.471 -0.986E-01 0.264 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0282
_refine_ls_wR_factor_gt          0.0246
_refine_ls_wR_factor_ref         0.0246
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                3034
_reflns_number_total             3315
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.89
_oxford_diffrn_Wilson_scale      8.80
_oxford_refine_ls_r_factor_ref   0.0269
_oxford_refine_ls_scale          0.3601(4)
_oxford_reflns_number_all        3297
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 5667
_cod_data_source_file            om100611p_si_002.cif
_cod_data_source_block           1^+^d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C11 H8 B1 Co2 F4 O5'
_cod_database_code               4066748