Structural Tungsten-Imido Chemistry: The Gas-Phase Structure of W(NBut)2(NHBut)2 and the Solid-State Structures of Novel Heterobimetallic W/N/M (M = Rh, Pd, Zn) Species
Hamid Choujaa; Samuel D. Cosham; Andrew L. Johnson; Graeme R. Kafka; Mary F. Mahon; Sarah L. Masters; Kieran C. Molloy; David W. H. Rankin; Heather E. Robertson; Derek A. Wann; Inorganic Chemistry 48 (2009) 2289–2299; doi:10.1021/ic8021134

data_4301611
_publ_section_title
;
Structural Tungsten-Imido Chemistry: The Gas-Phase Structure of
W(NBut)2(NHBut)2 and the Solid-State Structures of Novel Heterobimetallic
W/N/M (M = Rh, Pd, Zn) Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2289
_journal_page_last               2299
_journal_paper_doi               10.1021/ic8021134
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C32 H60 N4 Rh2 W'
_chemical_formula_sum            'C32 H60 N4 Rh2 W'
_chemical_formula_weight         890.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.1350(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.43800(10)
_cell_length_b                   11.6450(2)
_cell_length_c                   14.8040(2)
_cell_measurement_reflns_used    62935
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      40.22
_cell_measurement_theta_min      3.35
_cell_volume                     1710.05(4)
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 DENZO-SCALEPACK Z. Otwinowski and W. Minor, " 
 Processing of X-ray Diffraction Data Collected in Oscillation Mode ", 
 Methods in Enzymology, Volume 276: Macromolecular Crystallography, 
 part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
 SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). 
 Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, 
 Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 
;
_computing_structure_solution
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1133
_diffrn_reflns_av_sigmaI/netI    0.1264
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            62935
_diffrn_reflns_theta_full        40.22
_diffrn_reflns_theta_max         40.22
_diffrn_reflns_theta_min         2.98
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.335
_exptl_absorpt_correction_T_max  0.6509
_exptl_absorpt_correction_T_min  0.2139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
Sortav (Blessing 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.934
_refine_diff_density_min         -3.462
_refine_diff_density_rms         0.276
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.203(5)
_refine_ls_extinction_coef       0.0024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         21127
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1274
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                12701
_reflns_number_total             21127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8021134_si_002_2.cif
_cod_data_source_block           k04alj05
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4301611