Iron(III) complexes of 2-methyl-6-(pyrimidin-2-yl-hydrazonomethyl)-phenol as spin-crossover molecular materials
Yuan, Juan; Liu, Mei-Jiao; Liu, Cai-Ming; Kou, Hui-Zhong; Dalton Transactions  (2017) –; doi:10.1039/C7DT03233A

data_7044728
_publ_section_title
;
 Iron(III) complexes of 2-methyl-6-(pyrimidin-2-yl-hydrazonomethyl)-phenol
 as spin-crossover molecular materials
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03233A
_journal_year                    2017
_chemical_formula_moiety         'C24 H22 Fe N8 O2, Cl O4'
_chemical_formula_sum            'C24 H22 Cl Fe N8 O6'
_chemical_formula_weight         609.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_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   geom
_audit_creation_date             2017-10-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-20 deposited with the CCDC.
2017-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.747(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2935(3)
_cell_length_b                   18.4064(5)
_cell_length_c                   15.7629(5)
_cell_measurement_reflns_used    3883
_cell_measurement_temperature    293.00(10)
_cell_measurement_theta_max      72.3740
_cell_measurement_theta_min      3.7370
_cell_volume                     2607.58(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -129.00  20.00   1.00    2.00    --  -41.49   0.00  90.00  149
  2  \w     35.00  60.00   1.00    2.00    --   41.49-125.00  30.00   25
  3  \w     70.00 115.00   1.00    2.00    --   41.49  37.00-120.00   45
  4  \w    133.00 177.00   1.00   10.00    --  107.19  45.00 -90.00   44
  5  \w     75.00 175.00   1.00   10.00    --  107.19  77.00  60.00  100
  6  \w     34.00  92.00   1.00   10.00    --  107.19 -94.00 150.00   58
  7  \w    137.00 163.00   1.00   10.00    --  107.19 125.00 120.00   26
  8  \w     43.00 124.00   1.00   10.00    --  107.19 -45.00 -90.00   81
  9  \w     98.00 124.00   1.00   10.00    --  107.19 125.00 120.00   26
 10  \w     37.00  63.00   1.00   10.00    --  107.19-125.00 -90.00   26
 11  \w     78.00 114.00   1.00   10.00    --  107.19-125.00 -90.00   36
 12  \w    101.00 150.00   1.00   10.00    --  107.19  45.00-180.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0515406000
_diffrn_orient_matrix_UB_12      0.0603661000
_diffrn_orient_matrix_UB_13      0.0686890000
_diffrn_orient_matrix_UB_21      -0.1154306000
_diffrn_orient_matrix_UB_22      -0.0252332000
_diffrn_orient_matrix_UB_23      0.0485760000
_diffrn_orient_matrix_UB_31      0.1156682000
_diffrn_orient_matrix_UB_32      -0.0522120000
_diffrn_orient_matrix_UB_33      0.0560755000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9303
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         64.996
_diffrn_reflns_theta_min         3.765
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.078
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       rod
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         4432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0870
_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^)+67.9466P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3294
_refine_ls_wR_factor_ref         0.3340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3620
_reflns_number_total             4432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03233a2.cif
_cod_data_source_block           1-293K
_cod_database_code               7044728
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         c1h1n1o1Fe1Cl1
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C16(H16),
 C17(H17), C18(H18), C20(H20), C22(H22), C23(H23), C24(H24), N3(H3A), N7(H7A)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.218
_oxdiff_exptl_absorpt_empirical_full_min 0.731