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_7036857
_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_absolute_configuration ad
_chemical_formula_iupac          '[Ni (C23 H29 N5) (H2 O)] (Cl O4)2'
_chemical_formula_moiety         'C23 H31 N5 Ni O 2+, 2(Cl O4 1-)'
_chemical_formula_sum            'C23 H31 Cl2 N5 Ni O9'
_chemical_formula_weight         651.14
_chemical_name_systematic
;
aqua[N^1^,N^3^,2-trimethyl-2-(pyridin-2-yl)-N^1^,N^3^-bis(pyridin-
        2-ylmethyl)propane-1,3-diamine]nickel(II) perchlorate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5101(6)
_cell_length_b                   13.5280(4)
_cell_length_c                   12.2737(4)
_cell_measurement_reflns_used    4380
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      32.132
_cell_measurement_theta_min      3.685
_cell_volume                     2741.31(16)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
;
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0309
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11982
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         3.65
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1352
_exptl_crystal_recrystallization_method
'precipitation: wet methanol, diethyl ether, vapour diffusion, r.t., 4 d'
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    heteroxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         4759
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.3523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0754
_reflns_Friedel_coverage         0.75
_reflns_number_gt                4548
_reflns_number_total             4759
_reflns_threshold_expression     I>2\s(I)
_restr_special_details
;
 Equal-distance classes 1 and 2 were refined using a single free variable
 (d~2~ = 1.633 * d~1~) to make the O atoms fit a regular tetrahedron around Cl2.
;
_cod_data_source_file            c5dt02502h2.cif
_cod_data_source_block           mer-nil2
_cod_depositor_comments
'Adding full bibliography for 7036852--7036857.cif.'
_cod_database_code               7036857