Synthesis and dynamic behaviour of zwitterionic [M(η(6)-C6H5-BPh3)(coe)2] (M = Rh, Ir) cyclooctene complexes.
Pérez-Torrente, Jesús J; Angoy, Marta; Gómez-Bautista, Daniel; Palacios, Adrián; Jiménez, M Victoria; Modrego, F. Javier; Castarlenas, Ricardo; Lahoz, Fernando J.; Oro, Luis A.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14778–14786; doi:10.1039/c4dt02105c

data_7032013
_publ_section_title
;
 Synthesis and dynamic behaviour of zwitterionic
 [M(\h(6)-C6H5-BPh3)(coe)2] (M = Rh, Ir) cyclooctene complexes.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14778
_journal_page_last               14786
_journal_paper_doi               10.1039/c4dt02105c
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        'Prepared in the lab'
_chemical_formula_moiety         'C40 H48 B Ir, 0.25 (C H2 Cl2)'
_chemical_formula_sum            'C40.25 H48.5 B Cl0.5 Ir'
_chemical_formula_weight         753.03
_chemical_name_systematic
; 
 ? 
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.6882(12)
_cell_angle_beta                 79.8650(13)
_cell_angle_gamma                83.4888(11)
_cell_formula_units_Z            2
_cell_length_a                   9.0451(9)
_cell_length_b                   10.6166(10)
_cell_length_c                   18.0547(17)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.07
_cell_measurement_theta_min      2.33
_cell_volume                     1668.0(3)
_computing_cell_refinement       'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ENCIFER
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker APEX DUO 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  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17480
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.36
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    4.070
_exptl_absorpt_correction_T_max  0.5345
_exptl_absorpt_correction_T_min  0.4029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Multi-scan correction included in APEX2 package (Bruker AXS, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             761
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/Methanol'
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.176
_refine_diff_density_max         3.327
_refine_diff_density_min         -2.871
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         8303
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+5.9852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                7570
_reflns_number_total             8303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02105c4.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
'Adding full bibliography for 7032012--7032013.cif.'
_cod_original_formula_sum        'C40.25 H48.50 B Cl0.50 Ir'
_cod_database_code               7032013