The solid state structure and reactivity of NbCl(5) x (N,N'-dicyclohexylurea) in solution: evidence for co-ordinated urea dehydration to the relevant carbodiimide.
Aresta, Michele; Dibenedetto, Angela; Stufano, Paolo; Aresta, Brunella Maria; Maggi, Sabino; Pápai, Imre; Rokob, Tibor András; Gabriele, Bartolo; Dalton transactions (Cambridge, England : 2003) 39 (2010) 6985–6992; doi:10.1039/c001669a

data_7025551
_publ_section_title
;
 The solid state structure and reactivity of NbCl(5) x
 (N,N'-dicyclohexylurea) in solution: evidence for co-ordinated urea
 dehydration to the relevant carbodiimide.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6985
_journal_page_last               6992
_journal_paper_doi               10.1039/c001669a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C13 H24 Cl5 N2 Nb O'
_chemical_formula_sum            'C13 H24 Cl5 N2 Nb O'
_chemical_formula_weight         494.50
_chemical_melting_point          360
_chemical_name_common            NbCl5(N,N'-Dicyclohexylurea)
_chemical_name_systematic
;
NbCl5(N,N'-Dicyclohexylurea)
;
_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
_cell_angle_beta                 107.286(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.623(4)
_cell_length_b                   12.392(5)
_cell_length_c                   15.881(4)
_cell_measurement_reflns_used    78
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      5.02
_cell_volume                     1996.2(12)
_computing_cell_refinement       'DIRAX (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'COLLECT (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'DENZO and SCALEPAK(Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2008 (Burla , et al.2007)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_measurement_specimen_support fiber
_diffrn_radiation_collimation    'A 0.35 mm collimator was used'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18159
_diffrn_reflns_theta_full        24.40
_diffrn_reflns_theta_max         24.40
_diffrn_reflns_theta_min         5.01
_exptl_absorpt_coefficient_mu    1.274
_exptl_absorpt_correction_T_max  0.9275
_exptl_absorpt_correction_T_min  0.5154
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'SADABS (Brucker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 2990 Friedel pairs'
_refine_ls_abs_structure_Flack   0.17(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6417
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0394P)^2^+0.7258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                4866
_reflns_number_total             6417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c001669a.txt
_cod_data_source_block           NbCl5.(N,N'-dicyclohexylurea)
_cod_database_code               7025551