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_7049634
_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_compound_source        No
_chemical_formula_moiety         'C46 H38 Fe N6 O4, 3(C2 H3 N), 2(C24 H20 B)'
_chemical_formula_sum            'C100 H87 B2 Fe N9 O4'
_chemical_formula_weight         1556.25
_chemical_name_common            rac-2-MeCN-153K
_chemical_name_systematic        rac-2-MeCN-153K
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-06
_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                78.99(3)
_cell_angle_beta                 76.08(3)
_cell_angle_gamma                65.62(3)
_cell_formula_units_Z            2
_cell_length_a                   13.388(3)
_cell_length_b                   13.558(3)
_cell_length_c                   26.002(5)
_cell_measurement_reflns_used    12964
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      1.6225
_cell_volume                     4150.1(19)
_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 0.992
_diffrn_measured_fraction_theta_max 0.986
_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  0.0560
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            48409
_diffrn_reflns_point_group_measured_fraction_full 0.992
_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         0.811
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       block
_exptl_crystal_F_000             1636
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN and ether'
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1048
_refine_ls_number_reflns         18804
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0646
_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^)+(0.0508P)^2^+2.7203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1468
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16896
_reflns_number_total             18804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04893b2.cif
_cod_data_source_block           rac-2-MeCN-153K
_cod_depositor_comments
'Adding full bibliography for 7049629--7049635.cif.'
_cod_original_cell_volume        4150.4(18)
_cod_database_code               7049634
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   1.0000
_shelx_estimated_absorpt_t_min   0.8071
_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. Uiso/Uaniso restraints and constraints
Uanis(C95) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(N8) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C1(H1), C17(H17), C24(H24), C40(H40)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C16(H16A,H16B), C31(H31A,H31B), C39(H39A,H39B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), 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),
  C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61),
 C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70),
  C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C78(H78), C79(H79),
 C80(H80), C81(H81), C82(H82), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88),
  C90(H90), C91(H91), C92(H92), C93(H93), C94(H94)
3.d Idealised Me refined as rotating group:
 C95(H95A,H95B,H95C), C97(H97A,H97B,H97C), C99(H99A,H99B,H99C)
;
_shelx_res_checksum              95314
_olex2_submission_special_instructions 'No special instructions were received'