A novel crystal structure of {tris[4-(1<i>H</i>-pyrazol-3-yl-κ<i>N</i>^2^)-3-azabut-3-enyl]amine-κ<i>N</i>}iron(II) bis(tetrafluoridoborate) methanol monosolvate featuring a low-spin configuration
Struch, Niklas; Schnakenburg, Gregor; Lützen, Arne; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229615020409

data_2020293
_publ_section_title
;
 A novel crystal structure of
 {tris[4-(1<i>H</i>-pyrazol-3-yl-\k<i>N</i>^2^)-3-azabut-3-enyl]amine-\k<i>N</i>}iron(II)
 bis(tetrafluoridoborate) methanol monosolvate featuring a low-spin
 configuration
;
_journal_coeditor_code           EG3192
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615020409
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Fe (C18 H24 N10)] (B F4)2, C H4 O'
_chemical_formula_moiety         'C18 H24 Fe N10 2+, 2(B F4 -), C H4 O'
_chemical_formula_sum            'C19 H28 B2 F8 Fe N10 O'
_chemical_formula_weight         641.98
_chemical_name_systematic
'(Tris[4-(1<i>H</i>-pyrazol-3-yl-\k<i>N</i>^2^)-3-azabut-3-enyl]amine-\k<i>N</i>}iron(II) bis(tetrafluoridoborate) methanol monosolvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8634(7)
_cell_length_b                   12.6803(6)
_cell_length_c                   17.1975(9)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.903
_cell_measurement_theta_min      2.63
_cell_volume                     2587.0(2)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009) and
Mercury (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker X8 Kappa APEXII'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23363
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         3.338
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0800 before and 0.0551 after correction.
The Ratio of minimum to maximum transmission is 0.7899.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       needle
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.433
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2141 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   0.013(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6190
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+0.7928P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                5376
_reflns_number_total             6190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eg3192sup1.cif
_cod_data_source_block           I
_cod_database_code               2020293
_shelx_estimated_absorpt_t_min   0.876
_shelx_estimated_absorpt_t_max   0.973
_shelx_hkl_checksum              32420
_shelx_res_checksum              20842
_shelxl_version_number           20.13