Spin crossover and structural phase transition in homochiral and heterochiral Fe[(pybox)<sub>2</sub>]<sup>2+</sup> complexes.
Gao, Wan-Qing; Meng, Yin-Shan; Liu, Chun-Hua; Pan, Yao; Liu, Tao; Zhu, Yuan-Yuan; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6323–6327; doi:10.1039/c8dt04893b

data_7049633
_publ_section_title
;
 Spin crossover and structural phase transition in homochiral and
 heterochiral Fe[(pybox)<sub>2</sub>]<sup>2+</sup> complexes.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6323
_journal_page_last               6327
_journal_paper_doi               10.1039/c8dt04893b
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_compound_source        No
_chemical_formula_moiety         '2(C46 H38 Fe N6 O4), 4(Cl O4), 6(C2 H3 N)'
_chemical_formula_sum            'C104 H94 Cl4 Fe2 N18 O24'
_chemical_formula_weight         2233.47
_chemical_name_common            (S)-1-3MeCN-173K
_chemical_name_systematic        S-1-3MeCN-173K
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-17 deposited with the CCDC.    2019-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.051(4)
_cell_length_b                   21.637(4)
_cell_length_c                   25.014(5)
_cell_measurement_reflns_used    30696
_cell_measurement_temperature    173.0(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      1.2444
_cell_volume                     10311(4)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'MM007HF + CCD (Saturn724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            77662
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_min         1.244
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             4624
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN and ether'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 8190 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1375
_refine_ls_number_reflns         23629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+4.4879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1580
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                22124
_reflns_number_total             23629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04893b2.cif
_cod_data_source_block           S-1-3MeCN-173K
_cod_depositor_comments
'Adding full bibliography for 7049629--7049635.cif.'
_cod_database_code               7049633
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   1.0000
_shelx_estimated_absorpt_t_min   0.9011
_exptl_absorpt_special_details   SADABS
_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 Ternary CH refined with riding coordinates:
 C7(H7), C17(H17), C30(H30), C40(H40), C53(H53), C63(H63), C76(H76), C86(H86)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C16(H16A,H16B), C31(H31A,H31B), C39(H39A,H39B), C54(H54A,H54B),
 C62(H62A,H62B), C77(H77A,H77B), C85(H85A,H85B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43),
 C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
  C57(H57), C58(H58), C59(H59), C65(H65), C66(H66), C67(H67), C68(H68),
 C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C80(H80), C81(H81),
  C82(H82), C88(H88), C89(H89), C90(H90), C91(H91), C92(H92)
2.d Idealised Me refined as rotating group:
 C93(H93A,H93B,H93C), C95(H95A,H95B,H95C), C97(H97A,H97B,H97C), C99(H99A,H99B,
 H99C), C101(H10A,H10B,H10C), C103(H10D,H10E,H10F)
;
_shelx_res_checksum              9819
_olex2_submission_special_instructions 'No special instructions were received'