Synthesis, Characterization, and Reactivities of Molybdenum and Tungsten PONOP Pincer Complexes
Castro-Rodrigo, Ruth; Chakraborty, Sumit; Munjanja, Lloyd; Brennessel, William W.; Jones, William D.; Organometallics 35 (2016) 3124–; doi:10.1021/acs.organomet.6b00461

data_4086713
_publ_section_title
;
 Synthesis, Characterization, and Reactivities of Molybdenum and Tungsten
 PONOP Pincer Complexes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              3124
_journal_paper_doi               10.1021/acs.organomet.6b00461
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C24 H39 N O5 P2 W'
_chemical_formula_sum            'C24 H39 N O5 P2 W'
_chemical_formula_weight         667.35
_chemical_name_common            jonsc14
_chemical_name_systematic
; 
  (tBu-PONOP)W(CO)3 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 117.8272(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8572(16)
_cell_length_b                   13.1404(14)
_cell_length_c                   15.5556(16)
_cell_measurement_reflns_used    3889
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      38.24
_cell_measurement_theta_min      3.02
_cell_volume                     2685.7(5)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            99917
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        37.785
_diffrn_reflns_theta_max         38.656
_diffrn_reflns_theta_min         1.566
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.454
_exptl_absorpt_correction_T_max  0.4405
_exptl_absorpt_correction_T_min  0.3231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       wedge
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         5.176
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         14883
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+2.7286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13102
_reflns_number_total             14883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00461_si_003.cif
_cod_data_source_block           2c
_cod_database_code               4086713
_shelx_estimated_absorpt_t_min   0.470
_shelx_estimated_absorpt_t_max   0.536
_shelxl_version_number           2014-1
_shelx_res_checksum              86242
_shelx_hkl_checksum              83198