Fischer-Type Carbene Complexes of Tris(1,4-phenylene)amines and Tri(2-furyl)phosphine
Weststrate, Nora-ann; Fernández, Israel; Liles, David C.; van Jaarsveld, Nina; Lotz, Simon; Organometallics 34 (2015) 696–; doi:10.1021/om5008538

data_4085455
_publ_section_title
;
 Fischer-Type Carbene Complexes of Tris(1,4-phenylene)amines and
 Tri(2-furyl)phosphine
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              696
_journal_paper_doi               10.1021/om5008538
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C20 H13 O9 P W'
_chemical_formula_sum            'C20 H13 O9 P W'
_chemical_formula_weight         612.12
_chemical_name_systematic
;
 Pentacarbonyl-(ethoxy-(5-(di-2-furylphosphine)fur-2-yl)-methylidene)-
tungsten
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     intrinsic-phasing
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 93.651(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.3819(18)
_cell_length_b                   7.6045(3)
_cell_length_c                   13.7313(6)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      37.517
_cell_measurement_theta_min      2.725
_cell_volume                     4208.1(3)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
 ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
 Mercury (Macrae <i>et al</i>., 2008)
;
_computing_publication_material  'SHELXL-2013, PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXTL, SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXTS (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker kappa, Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'I\ms micro focus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       67
_diffrn_reflns_limit_h_min       -67
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            153596
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.317
_diffrn_reflns_theta_min         2.726
_exptl_absorpt_coefficient_mu    5.616
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.4770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' SADABS (Bruker, 2013)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.071
_refine_diff_density_max         2.425
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         10217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+3.7586P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                8601
_reflns_number_total             10217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5008538_si_002.cif
_cod_data_source_block           Cmplx_4b
_cod_depositor_comments
'Adding full bibliography for 4085452--4085456.cif.'
_cod_database_code               4085455
_shelxl_version_number           2013-2
_shelx_res_checksum              86325
_shelx_hkl_checksum              5086