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_7044732
_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 H21 Fe N8 O2, C O, O'
_chemical_formula_sum            'C25 H29 Fe N8 O4'
_chemical_formula_weight         561.41
_chemical_name_systematic
;
 ?
;
_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   mixed
_audit_creation_date             2017-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-08-13 deposited with the CCDC.
2017-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.848(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2328(3)
_cell_length_b                   16.0054(7)
_cell_length_c                   19.3465(11)
_cell_measurement_reflns_used    4604
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8550
_cell_measurement_theta_min      3.5450
_cell_volume                     2536.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14841
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.545
_diffrn_reflns_theta_min         3.349
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.73396
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       rod
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         6073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0734P)^2^+3.0543P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4552
_reflns_number_total             6073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03233a2.cif
_cod_data_source_block           4
_cod_database_code               7044732
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(O4A)=1-FVAR(1)
 Sof(O4)=FVAR(1)
3.a Riding coordinates:
 N3(H3)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C11(H11), C15(H15), C16(H16),
  C17(H17), C19(H19), C21(H21), C22(H22), C23(H23)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C24(H24A,H24B,H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'