An unusual example of a linearly coordinated acetone ligand in a six-coordinate iron(II) complex
Colin A. Kilner; Malcolm A. Halcrow; Acta Crystallographica Section C 62 (2006) m437–m439; doi:10.1107/S0108270106028903

data_2015560
_publ_section_title
;
 An unusual example of a linearly coordinated acetone ligand in a
 six-coordinate iron(II) complex
;
_journal_coeditor_code           GG3033
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m437
_journal_page_last               m439
_journal_paper_doi               10.1107/S0108270106028903
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'[Fe (C19 H25 N5) (C3 H6 O) (H2 O)2] (B F4)2, 2C3 H6 O'
_chemical_formula_moiety         'C22 H35 Fe N5 O3 2+, 2B F4 -, 2C3 H6 O'
_chemical_formula_sum            'C28 H47 B2 F8 Fe N5 O5'
_chemical_formula_weight         763.18
_chemical_name_systematic
;
diaqua(diethyl ether)[2,6-bis(3-tert-butylpyrazol-1-yl)pyridine]iron(II)
bis(tetrafluoroborate) diethyl ether disolvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 126.3230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.4575(4)
_cell_length_b                   12.78270(10)
_cell_length_c                   14.5598(4)
_cell_measurement_reflns_used    36356
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.80
_cell_volume                     3667.40(13)
_computing_cell_refinement       'DENZO--SMN (Otwinowski & Minor, 1997\\)'
_computing_data_collection       'COLLECT (Nonius, 1999\\)'
_computing_data_reduction        DENZO--SMN
_computing_molecular_graphics    'ORTEX (McArdle, 1995\\)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997\\)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997\\)'
_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 area-detector diffractometer'
_diffrn_measurement_method       '\w and \f'
_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  0.1305
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36356
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.745
_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 (1995), Acta Cryst. A51, 33-38
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular prism'
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.680
_refine_ls_extinction_coef       0.0057(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4190
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0459
_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^)+(0.062P)^2^+2.6971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1245
_reflns_number_gt                3718
_reflns_number_total             4190
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3033.cif
_cod_data_source_block           I
_cod_original_cell_volume        3667.40(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2015560
_cod_database_fobs_code          2015560