Spin switching in tris(8-aminoquinoline)iron(ii)(BPh<sub>4</sub>)<sub>2</sub>: quantitative guest-losing dependent spin crossover properties and single-crystal-to-single-crystal transformation.
Yang, Feng-Lei; Chen, Xin; Wu, Wen-Hao; Zhang, Jing-Hang; Zhao, Xiang-Mei; Shi, Yan-Hui; Shen, Fei; Dalton transactions (Cambridge, England : 2003) 48 (2018) 231–241; doi:10.1039/c8dt03584a

data_7048134
_publ_section_title
;
 Spin switching in
 tris(8-aminoquinoline)iron(ii)(BPh<sub>4</sub>)<sub>2</sub>: quantitative
 guest-losing dependent spin crossover properties and
 single-crystal-to-single-crystal transformation.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              231
_journal_page_last               241
_journal_paper_doi               10.1039/c8dt03584a
_journal_volume                  48
_journal_year                    2018
_chemical_formula_moiety         'C27 H24 Fe N6, 2(C24 H20 B)'
_chemical_formula_sum            'C75 H64 B2 Fe N6'
_chemical_formula_weight         1126.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-10-06
_audit_creation_method
; 
Olex2 1.2 
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) 
;
_audit_update_record
;
2018-10-26 deposited with the CCDC.
2018-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 129.397(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3622(6)
_cell_length_b                   34.072(2)
_cell_length_c                   19.1112(11)
_cell_measurement_reflns_used    3903
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      26.9906
_cell_measurement_theta_min      2.7550
_cell_volume                     6220.6(7)
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.,'
_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.,'
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      300.15
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'multiwire proportional'
_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  0.0891
_diffrn_reflns_av_unetI/netI     0.1208
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26034
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        23.997
_diffrn_reflns_theta_max         23.997
_diffrn_reflns_theta_min         2.760
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98079
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         9092
_refine_ls_number_restraints     751
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1666
_refine_ls_R_factor_gt           0.0992
_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^)+(0.0508P)^2^+0.0388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1475
_refine_ls_wR_factor_ref         0.1698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5529
_reflns_number_total             9092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03584a2.cif
_cod_data_source_block           p_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7048130--7048134.cif.'
_cod_database_code               7048134
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.893
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All N(H,H) groups 
2. Uiso/Uaniso restraints and constraints 
B2 \\sim C61A \\sim C60A \\sim C62A \\sim C59A \\sim C63A \\sim C58A \\sim C0AA 
\\sim C52A \\sim C75A \\sim C1AA \\sim C69A \\sim C65A \\sim C57A \\sim C53A 
\\sim C74A \\sim C72A \\sim C68A \\sim C66A \\sim C56A \\sim C54A \\sim C73A 
\\sim C67A \\sim C55A \\sim C52 \\sim C53 \\sim C57 \\sim C54 \\sim C56 \\sim 
C63 \\sim C64 \\sim C70 \\sim C55 \\sim C58 \\sim C62 \\sim C65 \\sim C69 \\sim 
C71 \\sim C75 \\sim C59 \\sim C61 \\sim C2CA \\sim C92 \\sim C72 \\sim C74 
\\sim C60 \\sim C4CA \\sim C73: within 2A with sigma of 0.02 and sigma for 
terminal atoms of 0.04 
C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim 
C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C69 \\sim C92 \\sim 
C2CA \\sim C4CA \\sim C70 \\sim C71 \\sim C75 \\sim C72 \\sim C73 \\sim C74: 
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 
C61A \\sim C60A \\sim C73A \\sim C74A \\sim C59A \\sim C62A \\sim C72A \\sim 
C0AA \\sim C66A \\sim C69A \\sim C75A \\sim B2 \\sim C63A \\sim C58A \\sim C56A 
\\sim C55A \\sim C57A \\sim C54A \\sim C53A \\sim C52A \\sim C68A \\sim C67A 
\\sim C65A \\sim C1AA: within 2A with sigma of 0.02 and sigma for terminal 
atoms of 0.04 
C75A \\sim C74A: within 2A with sigma of 0.002 and sigma for terminal atoms of 
0.004 
C75A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 
3. Others 
 Sof(C75A)=Sof(H75A)=FVAR(1) 
 Fixed Sof: C52(0.5) C53(0.5) H53(0.5) C54(0.5) H54(0.5) C55(0.5) H55(0.5) 
 C56(0.5) H56(0.5) C57(0.5) H57(0.5) C58(0.5) H58(0.5) C59(0.5) H59(0.5) 
 C60(0.5) H60(0.5) C61(0.5) H61(0.5) C62(0.5) H62(0.5) C63(0.5) C65(0.5) 
 H65(0.5) C69(0.5) H69(0.5) C61A(0.5) H61A(0.5) C60A(0.5) H60A(0.5) C73A(0.5) 
 H73A(0.5) C74A(0.5) H74A(0.5) C59A(0.5) H59A(0.5) C62A(0.5) H62A(0.5) 
 C72A(0.5) H72A(0.5) C0AA(0.5) C66A(0.5) H66A(0.5) C69A(0.5) H69A(0.5) 
 C63A(0.5) C58A(0.5) H58A(0.5) C56A(0.5) H56A(0.5) C55A(0.5) H55A(0.5) 
 C57A(0.5) H57A(0.5) C54A(0.5) H54A(0.5) C53A(0.5) H53A(0.5) C52A(0.5) C92(0.5) 
 H92(0.5) C68A(0.5) H68A(0.5) C2CA(0.5) H2CA(0.5) C67A(0.5) H67A(0.5) C4CA(0.5) 
 H4CA(0.5) C65A(0.5) H65A(0.5) C1AA(0.5) H1AA(0.5) C70(0.5) C71(0.5) H71(0.5) 
 C75(0.5) H75(0.5) C72(0.5) H72(0.5) C73(0.5) H73(0.5) C74(0.5) H74(0.5) 
4.a Secondary CH2 refined with riding coordinates: 
 N2(H2A,H2B), N3(H3A,H3B), N6(H6A,H6B) 
4.b Aromatic/amide H refined with riding coordinates: 
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), 
 C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), 
  C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), 
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), 
  C44(H44), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C55(H55), 
 C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C65(H65), 
  C69(H69), C61A(H61A), C60A(H60A), C73A(H73A), C74A(H74A), C59A(H59A), 
 C62A(H62A), C72A(H72A), C66A(H66A), C69A(H69A), C75A(H75A), C58A(H58A), 
 C56A(H56A), C55A(H55A), C57A(H57A), C54A(H54A), C53A(H53A), C92(H92), 
 C68A(H68A), C2CA(H2CA), C67A(H67A), C4CA(H4CA), C65A(H65A), C1AA(H1AA), 
 C71(H71), C75(H75), C72(H72), C73(H73), C74(H74) 
;
_olex2_submission_special_instructions 'No special instructions were received'