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_4085454
_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         'C34 H22 Br N O12 W2'
_chemical_formula_sum            'C34 H22 Br N O12 W2'
_chemical_formula_weight         1084.13
_chemical_name_systematic
;
 Decacarbonyl-\m-(4-bromophenyl-di-(4-(ethoxy-methylidene)-phenyl)-amino)-
di-tungsten
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     intrinsic-phasing
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90.262(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5309(13)
_cell_length_b                   22.5776(15)
_cell_length_c                   7.9946(5)
_cell_measurement_reflns_used    9564
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.465
_cell_measurement_theta_min      2.703
_cell_volume                     3525.3(4)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
;
 ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
 Mercury (Macrae <i>et al</i>., 2008)
;
_computing_publication_material  'SHELXL-2014, PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXTL, SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTS (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0598
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15782
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.520
_diffrn_reflns_theta_min         2.272
_exptl_absorpt_coefficient_mu    7.717
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.433
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.048
_refine_diff_density_max         3.201
_refine_diff_density_min         -1.701
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         15782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0277P)^2^+14.0388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                13593
_reflns_number_total             15782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5008538_si_002.cif
_cod_data_source_block           Cmplx_2b
_cod_depositor_comments
'Adding full bibliography for 4085452--4085456.cif.'
_cod_database_code               4085454
_shelxl_version_number           2014-1
_shelx_res_checksum              22037
_shelx_hkl_checksum              66593