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_4079095
_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         'C33 H27 B N3 P Pd S3'
_chemical_formula_sum            'C33 H27 B N3 P Pd S3'
_chemical_formula_weight         709.94
_chemical_name_common            Complex_6
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_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                97.541(2)
_cell_angle_beta                 102.928(2)
_cell_angle_gamma                109.843(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5022(3)
_cell_length_b                   10.2618(4)
_cell_length_c                   17.2908(6)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.35
_cell_volume                     1505.73(10)
_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 0.941
_diffrn_measured_fraction_theta_max 0.941
_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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13169
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.996
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+1.8900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                5877
_reflns_number_total             6569
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300482m_si_002.cif
_cod_data_source_block           (Complex_6)_az023_1_0m
_cod_original_cell_volume        1505.73(9)
_cod_database_code               4079095