A structurally-characterized NbCl5-NHC adduct
Marco Bortoluzzi; Eleonora Ferretti; Fabio Marchetti; Guido Pampaloni; Stefano Zacchini; Chem.Commun. 50 (2014) 4472–; doi:10.1039/C4CC01575D

data_7112263
_publ_section_title
;
 A structurally-characterized NbCl5-NHC adduct
;
_journal_name_full               Chem.Commun.
_journal_page_first              4472
_journal_paper_doi               10.1039/C4CC01575D
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C27 H36 Cl5 N2 Nb'
_chemical_formula_weight         658.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.682(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2250(17)
_cell_length_b                   17.760(3)
_cell_length_c                   17.334(3)
_cell_measurement_reflns_used    8942
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.090
_cell_measurement_theta_min      2.2935
_cell_volume                     3058.5(9)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0417
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28128
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  0.8761
_exptl_absorpt_correction_T_min  0.8352
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1262 (selected reflections only, before parameter refinement)
 R(int) =  0.0577 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            bright-orange
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.759
_refine_diff_density_min         -2.836
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         5338
_refine_ls_number_restraints     420
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.1310
_refine_ls_R_factor_gt           0.1049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+45.2159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1960
_refine_ls_wR_factor_ref         0.2121
_reflns_number_gt                4171
_reflns_number_total             5338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc01575d2.cif
_cod_data_source_block           p21n
_cod_original_cell_volume        3058.4(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7112263