Structural, Magnetic, and Mössbauer Spectral Study of the Electronic Spin-State Transition in [Fe{HC(3-Mepz)2(5-Mepz)}2](BF4)2
Daniel L. Reger; J. Derek Elgin; Elizabeth A. Foley; Mark D. Smith; Fernande Grandjean; Gary J. Long; Inorganic Chemistry 48 (2009) 9393–9401; doi:10.1021/ic901259e

data_4303308
_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
;
Structural, Magnetic, and M\"ossbauer Spectral Study of the Electronic
Spin-State Transition in [Fe{HC(3-Mepz)2(5-Mepz)}2](BF4)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9393
_journal_page_last               9401
_journal_paper_doi               10.1021/ic901259e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C26 H32 Fe N12, 2(B F4)'
_chemical_formula_sum            'C26 H32 B2 F8 Fe N12'
_chemical_formula_weight         742.11
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 108.3360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6343(5)
_cell_length_b                   13.0290(6)
_cell_length_c                   13.5476(6)
_cell_measurement_reflns_used    6807
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      25.020
_cell_measurement_theta_min      2.225
_cell_volume                     1614.23(13)
_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 0.999
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12235
_diffrn_reflns_theta_full        24.10
_diffrn_reflns_theta_max         24.10
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         2560
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0831P)^2^+0.8766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                2181
_reflns_number_total             2560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901259e_si_001_2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
 Marking atoms B1A, F1A, F2A, F3A, F4A, B1B, F1B, F2B, F3B, F4B,
 B1C, F1C, F2C, F3C, F4C as belonging to the same disorder assembly 'A'
 instead of 3 seperate ones ('A', 'B', 'C').

 Antanas Vaitkus,
 2017-01-24

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_cell_volume        1614.22(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4303308