Controlled ligand distortion and its consequences for structure, symmetry, conformation and spin-state preferences of iron(ii) complexes.
Kroll, Nicole; Theilacker, Kolja; Schoknecht, Marc; Baabe, Dirk; Wiedemann, Dennis; Kaupp, Martin; Grohmann, Andreas; Hörner, Gerald; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19232–19247; doi:10.1039/c5dt02502h

data_7036854
_publ_section_title
;
 Controlled ligand distortion and its consequences for structure,
 symmetry, conformation and spin-state preferences of iron(ii) complexes.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19232
_journal_page_last               19247
_journal_paper_doi               10.1039/c5dt02502h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_iupac          '[Fe(C F3 S O3)(C23 H27 N5)](C F3 S O3)'
_chemical_formula_moiety         'C24 H27 F3 Fe N5 O3 S 1+, C F3 O3 S 1-'
_chemical_formula_sum            'C25 H27 F6 Fe N5 O6 S2'
_chemical_formula_weight         727.49
_chemical_name_systematic
;(trifluoromethanesulfonato)[6-methyl-6-(pyridin-2-yl)-
1,4-bis(pyridin-2-ylmethyl)-1,4-diazepane]iron(II) trifluoromethanesulfonate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-17
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2014-06-17 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.124(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8155(3)
_cell_length_b                   17.6019(5)
_cell_length_c                   14.8106(4)
_cell_measurement_reflns_used    5907
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      32.5041
_cell_measurement_theta_min      3.4117
_cell_volume                     3062.66(14)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13451
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         3.42
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1488
_exptl_crystal_recrystallization_method
'precipitation: dichloromethane, diethyl ether, vapour diffusion, r.t., 5 d'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6006
_refine_ls_number_restraints     155
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.046
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+2.8354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.098
_reflns_number_gt                4989
_reflns_number_total             6006
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5dt02502h2.cif
_cod_data_source_block           mer-1-otf
_cod_depositor_comments
'Adding full bibliography for 7036852--7036857.cif.'
_cod_database_code               7036854