Utilizing the 8-Methoxycyclooct-4-en-1-ide Unit As a Hydrogen Atom Acceptor en Route to “Metal‒Borane Pincers”
Zech, Alexander; Haddow, Mairi F.; Othman, Hafiizah; Owen, Gareth R.; Organometallics 31 (2012) 6753–; doi:10.1021/om300482m

data_4079094
_publ_section_title
;
 Utilizing the 8-Methoxycyclooct-4-en-1-ide Unit As a Hydrogen Atom
 Acceptor en Route to &#x201C;Metal--Borane Pincers&#x201D;
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              6753
_journal_paper_doi               10.1021/om300482m
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C28 H24 B N2 P Pd S2, 0.07(C H2 Cl2)'
_chemical_formula_sum            'C28.07 H24.07 B Cl0.14 N2 P Pd S2'
_chemical_formula_weight         606.46
_chemical_name_common            Complex_5
_chemical_name_systematic
; 
 ? 
;
_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                97.1700(10)
_cell_angle_beta                 92.959(2)
_cell_angle_gamma                98.3360(10)
_cell_formula_units_Z            4
_cell_length_a                   8.5363(2)
_cell_length_b                   10.1753(3)
_cell_length_c                   30.8938(9)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.23
_cell_volume                     2627.65(13)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker ShelXTL'
_computing_publication_material  'Bruker ShelXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            46125
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.2080
_exptl_absorpt_correction_T_min  0.1669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1227
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.684
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         12050
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+2.8532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                9882
_reflns_number_total             12050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300482m_si_002.cif
_cod_data_source_block           (Complex_5)_az023
_cod_depositor_comments
;
 Removing the '_space_group_name_alt ' data item since it was not found
 in the core CIF dictionary and the same information was already provided in
 the official space group data items. No information was lost by removing this
 data item.

 Antanas Vaitkus,
 2017-03-06
;
_cod_database_code               4079094