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_4086714
_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_absolute_configuration ad
_chemical_formula_moiety         'C20 H31 N O5 P2 W'
_chemical_formula_sum            'C20 H31 N O5 P2 W'
_chemical_formula_weight         611.25
_chemical_name_common            jonlm21
_chemical_name_systematic        ' (iPr-PONOP)W(CO)3 '
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7399(19)
_cell_length_b                   11.323(2)
_cell_length_c                   19.424(4)
_cell_measurement_reflns_used    3911
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      38.34
_cell_measurement_theta_min      2.61
_cell_volume                     2362.1(8)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            73539
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        37.785
_diffrn_reflns_theta_max         38.588
_diffrn_reflns_theta_min         2.082
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.055
_exptl_absorpt_correction_T_max  0.4404
_exptl_absorpt_correction_T_min  0.2668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.866
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
; 
 Flack x determined using 5398 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.0091(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         12971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0172
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+0.0601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0360
_refine_ls_wR_factor_ref         0.0363
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                12495
_reflns_number_total             12971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00461_si_003.cif
_cod_data_source_block           2d
_cod_original_cell_volume        2362.1(7)
_cod_database_code               4086714
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.237
_shelx_estimated_absorpt_t_max   0.263
_shelx_res_checksum              41288
_shelx_hkl_checksum              73661