Topological Variations of the PDP Ligand and Its Prospects in Molybdenum(0) Dearomatization Agents
Benjamin K. Liebov; Caitlin E. Weigle; Kyle V. Keinath; Jennifer E. Leap; Robert D. Pike; Joseph M. Keane; Inorganic Chemistry 50 (2011) 4677–4679; doi:10.1021/ic200403t

data_4325261
_publ_section_title
;
 Topological Variations of the PDP Ligand and Its Prospects in
 Molybdenum(0) Dearomatization Agents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4677
_journal_page_last               4679
_journal_paper_doi               10.1021/ic200403t
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C20 H26 Cu N4, C2 H3 N, B F4, B F4'
_chemical_formula_sum            'C22 H29 B2 Cu F8 N5'
_chemical_formula_weight         600.66
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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
_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            4
_cell_length_a                   8.40340(10)
_cell_length_b                   12.4355(2)
_cell_length_c                   24.5737(3)
_cell_measurement_reflns_used    5932
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.00
_cell_measurement_theta_min      3.98
_cell_volume                     2567.96(6)
_computing_cell_refinement       'SAINTPLUS (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2004)'
_computing_data_reduction        SAINTPLUS
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'XSHELL (Bruker, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\w and \y'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            9482
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.931
_exptl_absorpt_correction_T_max  0.8751
_exptl_absorpt_correction_T_min  0.6782
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       purple
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0427P)^2^+0.6471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                3898
_reflns_number_total             4075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200403t_si_001_4.cif
_cod_data_source_block           p212121
_cod_database_code               4325261