Polymorphism-Dependent Spin-Crossover: Hysteretic Two-Step Spin Transition with an Ordered [HS-HS-LS] Intermediate Phase.
Luan, Jie; Zhou, Jian; Liu, Zhan; Zhu, Bowen; Wang, Huisi; Bao, Xin; Liu, Wei; Tong, Ming-Liang; Peng, Guo; Peng, Haonan; Salmon, Lionel; Bousseksou, Azzedine; Inorganic chemistry 54 (2015) 5145–5147; doi:10.1021/acs.inorgchem.5b00629

data_4346150
_publ_section_title
;
 Polymorphism-Dependent Spin-Crossover: Hysteretic Two-Step Spin
 Transition with an Ordered [HS-HS-LS] Intermediate Phase.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5145
_journal_page_last               5147
_journal_paper_doi               10.1021/acs.inorgchem.5b00629
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C18 H22 Fe N6 Se2'
_chemical_formula_sum            'C18 H22 Fe N6 Se2'
_chemical_formula_weight         536.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   39.457(6)
_cell_length_b                   17.701(3)
_cell_length_c                   8.9839(12)
_cell_measurement_reflns_used    2454
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.88
_cell_measurement_theta_min      2.98
_cell_volume                     6274.6(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0952
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11335
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.356
_diffrn_reflns_theta_min         2.301
_exptl_absorpt_coefficient_mu    4.217
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6160
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       plate
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Flack x determined using 1292 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5272
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0486P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1318
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_full    0.854
_reflns_Friedel_fraction_max     0.844
_reflns_number_gt                3761
_reflns_number_total             5272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00629_si_002.cif
_cod_data_source_block           1a_100K
_cod_original_cell_volume        6274.5(16)
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               4346150
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C11(H11A,H11B), C9(H9A,H9B), C26(H26A,H26B), C8(H8A,H8B),
 C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C22(H22), C13(H13), C2(H2), C16(H16), C1(H1), C20(H20), C4(H4),
 C21(H21), C14(H14), C3(H3), C15(H15)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              561
_shelx_hkl_checksum              87671
_olex2_submission_special_instructions 'No special instructions were received'