Synthesis and Characterization of Tungsten Alkylidene and Alkylidyne Complexes Supported by a New Pyrrolide-Centered Trianionic ONO3‒Pincer-Type Ligand
O’Reilly, Matthew E.; Nadif, Soufiane S.; Ghiviriga, Ion; Abboud, Khalil A.; Veige, Adam S.; Organometallics 33 (2014) 836–; doi:10.1021/om4009422

data_4082367
_publ_section_title
;
 Synthesis and Characterization of Tungsten Alkylidene and Alkylidyne
 Complexes Supported by a New Pyrrolide-Centered Trianionic
 ONO3--Pincer-Type Ligand
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              836
_journal_paper_doi               10.1021/om4009422
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C33 H44 N1 O3 W1, C19 H18 P1, C4 H10, O1'
_chemical_formula_sum            'C56 H72 N O4 P W'
_chemical_formula_weight         1037.97
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-08-21 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.866(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0367(14)
_cell_length_b                   14.5660(12)
_cell_length_c                   22.0816(18)
_cell_measurement_reflns_used    8780
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     5270.9(8)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Triumph'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56023
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.70
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.265
_exptl_absorpt_correction_T_max  0.9799
_exptl_absorpt_correction_T_min  0.7318
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.351
_refine_diff_density_min         -1.101
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         12092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+0.9083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0640
_reflns_number_gt                8643
_reflns_number_total             12092
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om4009422_si_002.cif
_cod_data_source_block           souf3
_cod_original_cell_volume        5270.9(7)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4082367