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_4131320
_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_formula_moiety         'C53 H67 Br1 Cl1 Fe1 N3 Nb1 O2 P3'
_chemical_formula_sum            'C53 H67 Br Cl Fe N3 Nb O2 P3'
_chemical_formula_weight         1135.16
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2015-04-16
_audit_creation_method           CRYSTALS_ver_14.61
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.9571(10)
_cell_length_b                   18.7784(9)
_cell_length_c                   25.3992(11)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     10472.6(8)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.065
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            79820
_diffrn_reflns_theta_full        29.450
_diffrn_reflns_theta_max         30.051
_diffrn_reflns_theta_min         1.603
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.444
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4688
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.130
_refine_diff_density_max         2.25
_refine_diff_density_min         -1.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         15249
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.0349543
_refine_ls_shift/su_mean         0.0013530
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ +18.07P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1045
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.1045
_reflns_limit_h_max              30
_reflns_limit_h_min              0
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                10480
_reflns_number_total             15249
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0675
_oxford_refine_ls_scale          0.0269237(12)
_oxford_reflns_number_all        15249
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'gc_02_113_0ma in Pbca'
_cod_data_source_file            ja7b04151_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        10472.6(5)
_cod_original_sg_symbol_Hall     '-P 2ac 2ab '
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        'C53 H67 Br1 Cl1 Fe1 N3 Nb1 O2 P3'
_cod_database_code               4131320