(1)H NMR spectroscopic elucidation in solution of the kinetics and thermodynamics of spin crossover for an exceptionally robust Fe(2+) complex.
Petzold, Holm; Djomgoue, Paul; Hörner, Gerald; Speck, J Matthäus; Rüffer, Tobias; Schaarschmidt, Dieter; Dalton transactions (Cambridge, England : 2003) 45 (2016) 13798–13809; doi:10.1039/c6dt01895e

data_7040054
_publ_section_title
;
 (1)H NMR spectroscopic elucidation in solution of the kinetics and
 thermodynamics of spin crossover for an exceptionally robust Fe(2+)
 complex.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13798
_journal_page_last               13809
_journal_paper_doi               10.1039/c6dt01895e
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'2(C32 H28 N6 Zn), 2(C32 H28 Fe N6), C4 H6 N2, 8(Cl O4)'
_chemical_formula_sum            'C132 H126 Cl8 Fe2 N26 O32 Zn2'
_chemical_formula_weight         3114.62
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-04-06 deposited with the CCDC.
2016-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.518(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   14.5861(3)
_cell_length_b                   13.0946(3)
_cell_length_c                   17.1156(3)
_cell_measurement_reflns_used    6481
_cell_measurement_temperature    110
_cell_measurement_theta_max      28.2430
_cell_measurement_theta_min      3.9920
_cell_volume                     3224.06(12)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14257
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.020
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 1941 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.021(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         5241
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+2.3431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.755
_reflns_Friedel_fraction_full    0.829
_reflns_Friedel_fraction_max     0.829
_reflns_number_gt                4802
_reflns_number_total             5241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01895e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7040051--7040055.cif.'
_cod_database_code               7040054
_shelxl_version_number           2013-4
_shelx_res_checksum              77757