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_7048130
_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), 1.5(C2 H3 N)'
_chemical_formula_sum            'C78 H68.5 B2 Fe N7.5'
_chemical_formula_weight         1188.37
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-10-04
_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                 128.432(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3870(6)
_cell_length_b                   34.330(2)
_cell_length_c                   18.8754(11)
_cell_measurement_reflns_used    5988
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.0189
_cell_measurement_theta_min      2.8185
_cell_volume                     6287.7(7)
_computing_cell_refinement
'CrysAlisPro, Oxford Diffraction Ltd.,Version 1.171.34.44'
_computing_data_collection
'CrysAlisPro, Oxford Diffraction Ltd.,Version 1.171.34.44'
_computing_data_reduction
'CrysAlisPro, Oxford Diffraction Ltd.,Version 1.171.34.44'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0537
_diffrn_reflns_av_unetI/netI     0.0971
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26836
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.824
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             2500
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   0.957
_exptl_transmission_factor_min   0.926
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     984
_refine_ls_number_reflns         12341
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0777
_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^)+(0.0303P)^2^+5.7027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8129
_reflns_number_total             12341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03584a2.cif
_cod_data_source_block           p
_cod_depositor_comments
'Adding full bibliography for 7048130--7048134.cif.'
_cod_original_formula_sum        'C78 H68.50 B2 Fe N7.50'
_cod_database_code               7048130
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.918
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C52A-C57A
 1.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C52 \\sim C57A \\sim C53 \\sim C54 \\sim C55A \\sim C56A: within 2A with sigma
of 0.002 and sigma for terminal atoms of 0.004
C57 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
C57A \\sim C52A \\sim C53A \\sim C54A \\sim C55A \\sim C56A: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C70A \\sim C75A \\sim C74A \\sim C73A \\sim C72A \\sim C71A: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C70A \\sim C71A \\sim C72A \\sim C73A \\sim C74A \\sim C75A: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C69A \\sim C68A \\sim C67A \\sim C66A \\sim C65A \\sim C64A: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C69 \\sim C68 \\sim C67 \\sim C66 \\sim C65: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
C69 \\sim C68 \\sim C67: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
N8 \\sim C77 \\sim C76: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04
C79 \\sim C78 \\sim N7: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04
4. Others
 Fixed Sof: C53(0.5) H53A(0.5) C56(0.5) H56A(0.5) C73(0.5) H73A(0.5) C71(0.5)
 H71A(0.5) C66(0.5) H66A(0.5) C74(0.5) H74A(0.5) C75(0.5) H75A(0.5) C72(0.5)
 H72A(0.5) C70(0.5) C64(0.5) H64A(0.5) C57(0.5) C67(0.5) H67A(0.5) C69(0.5)
 C68(0.5) H68A(0.5) C65(0.5) H65A(0.5) C55(0.5) H55A(0.5) C54(0.5) H54A(0.5)
 C52(0.5) H52A(0.5) B2(0.5) C64A(0.5) H64B(0.5) C66A(0.5) H66B(0.5) C71A(0.5)
 H71B(0.5) C68A(0.5) H69B(0.5) C70A(0.5) C67A(0.5) H67B(0.5) B0AA(0.5)
 C74A(0.5) H74B(0.5) C73A(0.5) H73B(0.5) C65A(0.5) H65B(0.5) C69A(0.5)
 C57A(0.5) C52A(0.5) H52B(0.5) C56A(0.5) H56B(0.5) C72A(0.5) H72B(0.5)
 C54A(0.5) H54B(0.5) C53A(0.5) H53B(0.5) C55A(0.5) H55B(0.5) C75A(0.5)
 H75B(0.5) N8(0.5) C77(0.5) C76(0.5) H76B(0.5) H76A(0.5) H76C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N2(H10A,H10B), N3(H10D,H10C), N6(H10E,H10F)
5.b Aromatic/amide H refined with riding coordinates:
 C16(H16A), C17(H17A), C7(H7A), C18(H18A), C3(H3A), C9(H9A), C1(H1A), C8(H8A),
 C13(H13A), C11(H11A), C21(H21A), C2(H2A), C12(H12A), C27(H27A), C23(H23A),
 C22(H22A), C25(H25A), C26(H26A), C48(H48A), C50(H50A), C44(H44A), C43(H43A),
 C51(H51A), C35(H35A), C40(H40A), C49(H49A), C47(H47A), C39(H39A), C33(H33A),
 C29(H29A), C30(H30A), C42(H42A), C41(H41A), C32(H32A), C38(H38A), C37(H37A),
 C36(H36A), C31(H31A), C53(H53A), C56(H56A), C73(H73A), C71(H71A), C66(H66A),
 C74(H74A), C75(H75A), C72(H72A), C64(H64A), C67(H67A), C68(H68A), C65(H65A),
 C55(H55A), C54(H54A), C52(H52A), C64A(H64B), C66A(H66B), C71A(H71B),
 C68A(H69B), C67A(H67B), C74A(H74B), C73A(H73B), C65A(H65B), C52A(H52B),
 C56A(H56B), C72A(H72B), C54A(H54B), C53A(H53B), C55A(H55B), C75A(H75B),
 C62(H62A), C61(H61A), C60(H60A), C58(H58A), C59(H59A)
5.c Idealised Me refined as rotating group:
 C79(H79A,H79B,H79C), C76(H76B,H76A,H76C)
;
_shelx_res_checksum              73797
_olex2_submission_special_instructions 'No special instructions were received'