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_4303591
_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), 1.5(C2 H3 N)'
_chemical_formula_sum            'C43 H40.5 B3 Cu2 F13 N17.5'
_chemical_formula_weight         1208.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_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                 103.0440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1714(3)
_cell_length_b                   42.3175(14)
_cell_length_c                   11.8649(4)
_cell_measurement_reflns_used    9624
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.001
_cell_measurement_theta_min      2.269
_cell_volume                     4975.2(3)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_molecular_graphics    various
_computing_publication_material  'SHELXTL Version 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0659
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            46356
_diffrn_reflns_theta_full        24.13
_diffrn_reflns_theta_max         24.13
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    0.958
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2444
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         8051
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                6129
_reflns_number_total             8051
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901352p_si_001_4.cif
_cod_data_source_block           Cuacn
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'C43 H40.50 B3 Cu2 F13 N17.50'
_cod_database_code               4303591