Heterobimetallic Complexes Comprised of Nb and Fe: Isolation of a Coordinatively Unsaturated Nb<sup>III</sup>/Fe<sup>0</sup> Bimetallic Complex Featuring a Nb≡Fe Triple Bond.
Culcu, Gursu; Iovan, Diana A.; Krogman, Jeremy P.; Wilding, Matthew J. T.; Bezpalko, Mark W.; Foxman, Bruce M.; Thomas, Christine M.; Journal of the American Chemical Society 139 (2017) 9627–9636; doi:10.1021/jacs.7b04151

data_4131321
_publ_section_title
;
 Heterobimetallic Complexes Comprised of Nb and Fe: Isolation of a
 Coordinatively Unsaturated Nb<sup>III</sup>/Fe<sup>0</sup> Bimetallic
 Complex Featuring a Nb\\tb Fe Triple Bond.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9627
_journal_page_last               9636
_journal_paper_doi               10.1021/jacs.7b04151
_journal_volume                  139
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C47 H53 Cl3 F3 N3 Nb1 O3 P3 S1'
_chemical_formula_sum            'C47 H53 Cl3 F3 N3 Nb O3 P3 S'
_chemical_formula_weight         1089.20
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-11
_audit_creation_method           CRYSTALS_ver_14.61_build_00000
_cell_angle_alpha                90
_cell_angle_beta                 110.611(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0896(7)
_cell_length_b                   20.9802(13)
_cell_length_c                   11.1696(7)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    120
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     2432.4(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            34235
_diffrn_reflns_theta_full        27.593
_diffrn_reflns_theta_max         28.157
_diffrn_reflns_theta_min         1.941
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120.000
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.38
_refine_diff_density_min         -2.41
_refine_ls_abs_structure_details 'Flack (1983), 4420 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         10487
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.0002665
_refine_ls_shift/su_mean         0.0000154
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.14P)^2^ + 0.17P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1597
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1597
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              27
_reflns_limit_k_min              -21
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                9768
_reflns_number_total             10487
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.31
_oxford_diffrn_Wilson_scale      57.17
_oxford_refine_ls_r_factor_ref   0.0632
_oxford_refine_ls_scale          0.14998(8)
_oxford_reflns_number_all        10487
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'gc_05_456_0m in P2(1)'
_cod_data_source_file            ja7b04151_si_002.cif
_cod_data_source_block           5
_cod_original_sg_symbol_Hall     'P 2yb '
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C47 H53 Cl3 F3 N3 Nb1 O3 P3 S1'
_cod_database_code               4131321