Partial Nitrogen Atom Transfer: A New Synthetic Tool to Design Single-Molecule Magnets.
Ding, Mei; Rouzières, Mathieu; Losovyj, Yaroslav; Pink, Maren; Clérac, Rodolphe; Smith, Jeremy M.; Inorganic chemistry 54 (2015) 9075–9080; doi:10.1021/acs.inorgchem.5b01455

data_4344102
_publ_section_title
;
 Partial Nitrogen Atom Transfer: A New Synthetic Tool to Design
 Single-Molecule Magnets.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9075
_journal_page_last               9080
_journal_paper_doi               10.1021/acs.inorgchem.5b01455
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C69 H77 B Fe N7 V, 6 (C4 H8 O)'
_chemical_formula_sum            'C93 H125 B Fe N7 O6 V'
_chemical_formula_weight         1554.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   19.5861(9)
_cell_length_b                   19.5861(9)
_cell_length_c                   76.340(4)
_cell_measurement_reflns_used    9665
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      12.41
_cell_measurement_theta_min      2.23
_cell_volume                     25362(2)
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2013)'
_computing_publication_material  'SHELXTL (Bruker, 2013)'
_computing_structure_refinement  'SHELXTL (Bruker, 2012)'
_computing_structure_solution    'SHELXTL (Bruker, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
'0.5 degree frames measured for 2 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'silicon  1 1 1 and 3 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1406
_diffrn_reflns_av_sigmaI/netI    0.0672
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       95
_diffrn_reflns_limit_l_min       -95
_diffrn_reflns_number            110189
_diffrn_reflns_theta_full        14.98
_diffrn_reflns_theta_max         14.98
_diffrn_reflns_theta_min         0.76
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.9907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick; 2014'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10008
_exptl_crystal_size_max          0.051
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.008
_refine_diff_density_max         1.260
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5784
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1907
_refine_ls_R_factor_gt           0.1087
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1968P)^2^+177.9393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2986
_refine_ls_wR_factor_ref         0.3681
_reflns_number_gt                3091
_reflns_number_total             5784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01455_si_002.cif
_cod_data_source_block           s14004
_cod_depositor_comments          'Adding full bibliography for 4344102.cif.'
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               4344102