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_7049635
_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        none
_chemical_formula_moiety         '4(C46 H38 Fe N6 O4), 8(C24 H20 B)'
_chemical_formula_sum            'C376 H312 B8 Fe4 N24 O16'
_chemical_formula_weight         5732.38
_chemical_name_common            S-2-MeCN-153K
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-14 deposited with the CCDC.    2019-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.46(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.154(5)
_cell_length_b                   26.161(5)
_cell_length_c                   26.794(5)
_cell_measurement_reflns_used    53173
_cell_measurement_temperature    153.0(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      1.3429
_cell_volume                     16093(6)
_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  'XH (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0744
_diffrn_reflns_av_unetI/netI     0.1227
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            100918
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.77
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6016
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN and ether'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
The disordered solvent molecules cannot be modeled and were treated 
by SQUEEZE,PLATON.
There are total 176e per unit cell were accumulated which corresponds 
to 28e per Fe(II) uint. The 22e might come from a 
acetonitrile molecule and were not included in the formula.
;
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.046(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3853
_refine_ls_number_reflns         52000
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.1052
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+29.4053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2261
_refine_ls_wR_factor_ref         0.2467
_reflns_number_gt                39265
_reflns_number_total             52000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt04893b2.cif
_cod_data_source_block           1879557
_cod_depositor_comments
'Adding full bibliography for 7049629--7049635.cif.'
_cod_database_code               7049635
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(B5) \\sim Ueq, Uanis(C133) \\sim Ueq, Uanis(C353) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C7(H7), C17(H17), C30(H30), C40(H40), C53(H53), C63(H63), C76(H76), C86(H86),
 C99(H99), C109(H109), C122(H122), C132(H132), C145(H145), C155(H155),
 C168(H168), C178(H178)
3.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), C100(H10A,H10B), C108(H10C,
 H10D), C123(H12A,H12B), C131(H13A,H13B), C146(H14A,H14B), C154(H15A,H15B),
 C169(H16C,H16D), C177(H17A,H17B)
3.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), C94(H94),
 C95(H95), C96(H96), C97(H97), C98(H98), C103(H103), C104(H104), C105(H105),
 C111(H111), C112(H112), C113(H113), C114(H114), C115(H115), C117(H117),
 C118(H118), C119(H119), C120(H120), C121(H121), C126(H126), C127(H127),
 C128(H128), C134(H134), C135(H135), C136(H136), C137(H137), C138(H138),
 C140(H140), C141(H141), C142(H142), C143(H143), C144(H144), C149(H149),
 C150(H150), C151(H151), C157(H157), C158(H158), C159(H159), C160(H160),
 C161(H161), C163(H163), C164(H164), C165(H165), C166(H166), C167(H167),
 C172(H172), C173(H173), C174(H174), C180(H180), C181(H181), C182(H182),
 C183(H183), C184(H184), C186(H186), C187(H187), C188(H188), C189(H189),
 C190(H190), C192(H192), C193(H193), C194(H194), C195(H195), C196(H196),
 C198(H198), C199(H199), C200(H200), C201(H201), C202(H202), C204(H204),
 C205(H205), C206(H206), C207(H207), C208(H208), C210(H210), C211(H211),
 C212(H212), C213(H213), C214(H214), C216(H216), C217(H217), C218(H218),
 C219(H219), C220(H220), C222(H222), C223(H223), C224(H224), C225(H225),
 C226(H226), C228(H228), C229(H229), C230(H230), C231(H231), C232(H232),
 C234(H234), C235(H235), C236(H236), C237(H237), C238(H238), C240(H240),
 C241(H241), C242(H242), C243(H243), C244(H244), C246(H246), C247(H247),
 C248(H248), C249(H249), C250(H250), C252(H252), C253(H253), C254(H254),
 C255(H255), C256(H256), C258(H258), C259(H259), C260(H260), C261(H261),
 C262(H262), C264(H264), C265(H265), C266(H266), C267(H267), C268(H268),
 C270(H270), C271(H271), C272(H272), C273(H273), C274(H274), C276(H276),
 C277(H277), C278(H278), C279(H279), C280(H280), C282(H282), C283(H283),
 C284(H284), C285(H285), C286(H286), C288(H288), C289(H289), C290(H290),
 C291(H291), C292(H292), C294(H294), C295(H295), C296(H296), C297(H297),
 C298(H298), C300(H300), C301(H301), C302(H302), C303(H303), C304(H304),
 C306(H306), C307(H307), C308(H308), C309(H309), C310(H310), C312(H312),
 C313(H313), C314(H314), C315(H315), C316(H316), C318(H318), C319(H319),
 C320(H320), C321(H321), C322(H322), C324(H324), C325(H325), C326(H326),
 C327(H327), C328(H328), C330(H330), C331(H331), C332(H332), C333(H333),
 C334(H334), C336(H336), C337(H337), C338(H338), C339(H339), C340(H340),
 C342(H342), C343(H343), C344(H344), C345(H345), C346(H346), C348(H348),
 C349(H349), C350(H350), C351(H351), C352(H352), C354(H354), C355(H355),
 C356(H356), C357(H357), C358(H358), C360(H360), C361(H361), C362(H362),
 C363(H363), C364(H364), C366(H366), C367(H367), C368(H368), C369(H369),
 C370(H370), C372(H372), C373(H373), C374(H374), C375(H375), C376(H376)
;
_olex2_submission_special_instructions 'No special instructions were received'