Vanadium–iron complexes featuring metal–metal multiple bonds
Kuppuswamy, Subramaniam; Powers, Tamara M.; Krogman, Jeremy P.; Bezpalko, Mark W.; Foxman, Bruce M.; Thomas, Christine M.; Chemical Science 4 (2013) 3557–; doi:10.1039/c3sc51337h

data_1514804
_publ_section_title
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 Vanadium--iron complexes featuring metal--metal multiple bonds
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_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              3557
_journal_paper_doi               10.1039/c3sc51337h
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'C48 H60 Fe1 N3 P4 V1'
_chemical_formula_sum            'C48 H60 Fe N3 P4 V'
_chemical_formula_weight         909.71
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             13-02-14
_audit_creation_method           CRYSTALS_ver_14.41
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   16.3841(5)
_cell_length_b                   16.3841(5)
_cell_length_c                   22.8729(9)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     5317.4(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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.061
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5179
_diffrn_reflns_theta_full        30.006
_diffrn_reflns_theta_max         30.006
_diffrn_reflns_theta_min         3.059
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.190
_platon_squeeze_details
;
During the structure solution, electron density difference maps 
revealed that there was a disordered solvent molecule which 
could not be successfully modeled.  The solvate was 
highly disordered due to symmetry in a volume of 949 cubic angstroms per unit cell.  
It appeared that the cavity area contained ca. 2 ether molecules, 
located near (0, 0, 0). Modeling with or without restraints was 
unsuccessful, as was step by step acquisition of peaks using 
successive electron density difference maps.  Thus, the structure 
factors were modified using the PLATON SQUEEZE technique, 
in order to produce a "solvate-free" structure factor set.  
PLATON reported a total electron density of 70 e- per unit 
cell, likely representing two ether molecules, 
consistent with our earlier observations.  Use of the SQUEEZE 
technique resulted in a decrease of ca. 1.6 % in R.
;
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         5179
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.0011931
_refine_ls_shift/su_mean         0.0000678
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 3.29P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0993
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0993
_reflns_limit_h_max              0
_reflns_limit_h_min              -19
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                4019
_reflns_number_total             5179
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.29
_oxford_diffrn_Wilson_scale      151.57
_oxford_refine_ls_r_factor_ref   0.0446
_oxford_refine_ls_scale          0.08230(2)
_oxford_reflns_number_all        5179
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'SK_747_0m in P-3c1'
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  22,X'S) H   (  23,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  33,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 163,X'S) H   ( 162,X'S) H   ( 161,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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_cod_data_source_file            c3sc51337h.txt
_cod_data_source_block           4
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
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_cod_original_formula_sum        'C48 H60 Fe1 N3 P4 V1'
_cod_database_code               1514804