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_7036853
_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 H3 C N)(C23 H27 N5)](B{C6 H5}4)2'
_chemical_formula_moiety         'C25 H30 Fe N6 2+, 2(C24 H20 B 1-)'
_chemical_formula_sum            'C73 H70 B2 Fe N6'
_chemical_formula_weight         1108.82
_chemical_name_systematic
;acetonitrile[6-methyl-6-(pyridin-2-yl)-1,4-bis(pyridin-2-ylmethyl)-
        1,4-diazepane]iron(II) tetraphenylborate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 90.4960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0919(2)
_cell_length_b                   33.6364(5)
_cell_length_c                   14.6502(2)
_cell_measurement_reflns_used    11196
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.287
_cell_measurement_theta_min      3.276
_cell_volume                     5958.42(16)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
;
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5435
_diffrn_detector_type            'Agilent Atlas'
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova (Single Source)'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46761
_diffrn_reflns_theta_full        67.5
_diffrn_reflns_theta_max         67.5
_diffrn_reflns_theta_min         2.63
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'Agilent Nova'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.399
_exptl_absorpt_correction_T_max  0.8131
_exptl_absorpt_correction_T_min  0.6084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2344
_exptl_crystal_recrystallization_method
'precipitation: acetonitrile, diethyl ether, layering, r.t., 7 d'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         10755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+1.4804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                8845
_reflns_number_total             10755
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5dt02502h2.cif
_cod_data_source_block           mer-1-mecn_cu-478
_cod_depositor_comments
'Adding full bibliography for 7036852--7036857.cif.'
_cod_database_code               7036853