Monofluoride Bridged, Binuclear Metallacycles of First Row Transition Metals Supported by Third Generation Bis(1-pyrazolyl)methane Ligands: Unusual Magnetic Properties
Daniel L. Reger; Elizabeth A. Foley; Russell P. Watson; Perry J. Pellechia; Mark D. Smith; Fernande Grandjean; Gary J. Long; Inorganic Chemistry 48 (2009) 10658–10669; doi:10.1021/ic901352p

data_4303592
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of South Carolina
Columbia, South Carolina 29208
USA
;
_publ_contact_author_email       reger@mail.chem.sc.edu
_publ_contact_author_fax         '1 803 777 9521'
_publ_contact_author_name        'Professor Daniel L. Reger'
_publ_contact_author_phone       '1 803 777 2587'
_publ_section_title
;
Monofluoride Bridged, Binuclear Metallacycles of First Row Transition
Metals Supported by Third Generation Bis(1-pyrazolyl)methane Ligands:
Unusual Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10658
_journal_page_last               10669
_journal_paper_doi               10.1021/ic901352p
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C40 H36 Cu2 F1 N16, 3(B F4), 2.25(C3 H6 O)'
_chemical_formula_sum            'C46.75 H49.5 B3 Cu2 F13 N16 O2.25'
_chemical_formula_weight         1278.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.8870(10)
_cell_angle_beta                 76.7830(10)
_cell_angle_gamma                68.0040(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3642(4)
_cell_length_b                   13.8264(4)
_cell_length_c                   16.4223(5)
_cell_measurement_reflns_used    7710
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      26.262
_cell_measurement_theta_min      2.306
_cell_volume                     2738.35(14)
_computing_cell_refinement       'SAINT+ NT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART NT V5.625 (Bruker, 1998)'
_computing_data_reduction        'SAINT+ NT V6.22'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0671
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28446
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         11211
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                8072
_reflns_number_total             11211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901352p_si_001_5.cif
_cod_data_source_block           Cuacetone
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C46.75 H49.50 B3 Cu2 F13 N16 O2.25'
_cod_database_code               4303592