The spin-states and spin-crossover behaviour of iron(II) complexes of 2,6-dipyrazol-1-ylpyrazine derivatives
Jérôme Elhaïk; Victoria A. Money; Simon A. Barrett; Colin A. Kilner; Ivana Radosavljevic Evans; Malcolm A. Halcrow; Dalton Trans.  (2003) 2053–2060; doi:10.1039/b210368k

data_7012356
_publ_section_title
;
 The spin-states and spin-crossover behaviour of iron(II) complexes of
 2,6-dipyrazol-1-ylpyrazine derivatives
;
_journal_issue                   10
_journal_name_full               'Dalton Trans.'
_journal_page_first              2053
_journal_page_last               2060
_journal_paper_doi               10.1039/b210368k
_journal_year                    2003
_chemical_formula_moiety         'C56 H56 B2 F8 Fe N12, 2[B F4], 5[C H3 N O2]'
_chemical_formula_sum            'C61 H71 B2 F8 Fe N17 O10'
_chemical_formula_weight         1431.82
_chemical_name_common
;
Bis(2,6-bis(3-(2,4,6-trimethylphenyl)pyrazol-1-
yl)pyrazine)iron(ii) ditetrafluoroborate pentakis-nitromethane solvate
;
_chemical_name_systematic
; 
Bis[2,6-bis(3-{2,4,6-trimethylphenyl}pyrazol-1-yl)pyrazine]iron(II) 
ditetrafluoroborate pentakis-nitromethane solvate
;
_space_group_IT_number           152
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.1838(1)
_cell_length_b                   15.1838(1)
_cell_length_c                   24.9779(2)
_cell_measurement_reflns_used    89750
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      1.55
_cell_volume                     4987.09(6)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'Area detector 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  0.1573
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            89750
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  0.9101
_exptl_absorpt_correction_T_min  0.8070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_crystal_colour            'Dark brown'
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(19)
_refine_ls_extinction_coef       0.0051(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         7623
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0948P)^2^+3.0942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1603
_reflns_number_gt                7105
_reflns_number_total             7623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210368k.txt
_cod_data_source_block           je28
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
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 31 21'
_cod_database_code               7012356