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_7049629
_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         '3(C46 H38 Fe N6 O4), 6(Cl O4), 9(C2 H3 N)'
_chemical_formula_sum            'C156 H141 Cl6 Fe3 N27 O36'
_chemical_formula_weight         3350.20
_chemical_name_common            (S)-1-3MeCN-153K
_chemical_name_systematic        (S)-1-3MeCN-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   mixed
_audit_creation_date             2019-04-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-08 deposited with the CCDC.    2019-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.91(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.120(4)
_cell_length_b                   21.609(4)
_cell_length_c                   21.015(4)
_cell_measurement_reflns_used    26063
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      1.1943
_cell_volume                     7742(3)
_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      153.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_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  0.0402
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            66419
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         2.176
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             3468
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile and ether'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 11820 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1837
_refine_ls_number_reflns         35105
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0655
_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^)+(0.1125P)^2^+2.0053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1753
_refine_ls_wR_factor_ref         0.1825
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                32438
_reflns_number_total             35105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04893b2.cif
_cod_data_source_block           1879551
_cod_depositor_comments
'Adding full bibliography for 7049629--7049635.cif.'
_cod_original_cell_volume        7743(3)
_cod_database_code               7049629
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   1.0000
_shelx_estimated_absorpt_t_min   0.7102
_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. Restrained distances
 Cl1-O13 \\sim Cl1-O14 \\sim Cl1-O15 \\sim Cl1-O16
 with sigma of 0.01
 O13-O14 \\sim O14-O15 \\sim O15-O16 \\sim O16-O13
 with sigma of 0.02
 Cl2-O17 \\sim Cl2-O18 \\sim Cl2-O19 \\sim Cl2-O20
 with sigma of 0.01
 O17-O18 \\sim O18-O19 \\sim O19-O20 \\sim O20-O17
 with sigma of 0.02
 Cl3-O21 \\sim Cl3-O22 \\sim Cl3-O23 \\sim Cl3-O24
 with sigma of 0.01
 O21-O22 \\sim O22-O23 \\sim O23-O24 \\sim O24-O21
 with sigma of 0.02
 Cl4-O25 \\sim Cl4-O26 \\sim Cl4-O27 \\sim Cl4-O28
 with sigma of 0.01
 O25-O26 \\sim O26-O27 \\sim O27-O28 \\sim O28-O25
 with sigma of 0.02
 Cl5-O29 \\sim Cl5-O30 \\sim Cl5-O31 \\sim Cl5-O32
 with sigma of 0.01
 O29-O30 \\sim O30-O31 \\sim O31-O32 \\sim O32-O29
 with sigma of 0.02
 Cl6-O33 \\sim Cl6-O34 \\sim Cl6-O35 \\sim Cl6-O36
 with sigma of 0.01
 O33-O34 \\sim O34-O35 \\sim O35-O36 \\sim O36-O33
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O30)
\\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(O34) \\sim Ueq,
Uanis(O36) \\sim Ueq, Uanis(N25) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Riding coordinates:
 C139(H13C,H13D,H13E), C141(H14A,H14B,H14C), C143(H14D,H14E,H14F), C145(H14G,
 H14H,H14I), C147(H14J,H14K,H14L), C149(H14M,H14N,H14O), C151(H15A,H15B,H15C),
 C153(H15D,H15E,H15F), C155(H15G,H15H,H15I)
4.b 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)
4.c 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)
4.d Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C11(H11), C34(H34), C35(H35), C36(H36), C6(H6), C5(H5),
 C4(H4), C3(H3), C2(H2), C23(H23), C22(H22), C21(H21), C20(H20), C19(H19),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C57(H57), C58(H58), C59(H59), C80(H80), C81(H81),
 C82(H82), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C65(H65), C66(H66),
  C67(H67), C68(H68), C69(H69), C75(H75), C74(H74), C73(H73), C72(H72),
 C71(H71), C88(H88), C89(H89), C90(H90), C91(H91), C92(H92), C103(H103),
 C104(H104), C105(H105), C128(H128), C127(H127), C126(H126), C94(H94), C95(H95),
  C96(H96), C97(H97), C98(H98), C111(H111), C112(H112), C113(H113), C114(H114),
 C115(H115), C121(H121), C120(H120), C119(H119), C118(H118), C117(H117),
 C138(H138), C137(H137), C136(H136), C135(H135), C134(H134)
4.e Fitted hexagon refined as free rotating group:
 N2(C14,C13,C12,C11,C10), N5(C33,C34,C35,C36,C37), C1(C6,C5,C4,C3,C2), C18(C23,
 C22,C21,C20,C19), C24(C25,C26,C27,C28,C29), C41(C42,C43,C44,C45,C46), N8(C56,
 C57,C58,C59,C60), N11(C79,C80,C81,C82,C83), C47(C48,C49,C50,C51,C52), C64(C65,
 C66,C67,C68,C69), C70(C75,C74,C73,C72,C71), C87(C88,C89,C90,C91,C92), N14(C102,
 C103,C104,C105,C106), N17(C129,C128,C127,C126,C125), C93(C94,C95,C96,C97,C98),
 C110(C111,C112,C113,C114,C115), C116(C121,C120,C119,C118,C117), C138(C137,C136,
 C135,C134,C133)
;
_shelx_res_checksum              32310
_olex2_submission_special_instructions 'No special instructions were received'