A linear trinuclear ferrous single molecule magnet.
Liu, Shihao; Deng, Yi-Fei; Li, Chang'An; Chang, Xiaoyong; Zhang, Yuan-Zhu; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16704–16708; doi:10.1039/c8dt03410a

data_7047873
_publ_section_title
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 A linear trinuclear ferrous single molecule magnet.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16704
_journal_page_last               16708
_journal_paper_doi               10.1039/c8dt03410a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C50 H44 Fe3 N8 O6, 2(C24 H20 B), 2(C H4 O)'
_chemical_formula_sum            'C100 H92 B2 Fe3 N8 O8'
_chemical_formula_weight         1722.98
_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   mixed
_audit_creation_date             2017-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-07-17 deposited with the CCDC.
2018-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                72.543(3)
_cell_angle_beta                 68.325(3)
_cell_angle_gamma                69.161(3)
_cell_formula_units_Z            1
_cell_length_a                   11.5264(11)
_cell_length_b                   14.2406(14)
_cell_length_c                   15.0986(15)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.35
_cell_volume                     2111.5(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9512
_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         27.559
_diffrn_reflns_theta_min         2.052
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1444 before and 0.0798 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1521 before and 0.0878 after correction.
 The Ratio of minimum to maximum transmission is 0.42.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 54073 reflections, Rint = 0.1062
 (21139 with I > 3sig(I), Rint = 0.0718)
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         9512
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0573P)^2^+3.3185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7708
_reflns_number_total             9512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03410a2.cif
_cod_data_source_block           mo_shihao26_0m_4
_cod_depositor_comments          'Adding full bibliography for 7047873.cif.'
_cod_database_code               7047873
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.3131(9)
 0.6869(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 O3-H3
 0.87 with sigma of 0.01
 C25-H3
 1.905563 with sigma of 0.02
 Fe1-H3
 2.808112 with sigma of 0.02
 H5-H3
 2.2 with sigma of 0.04
 H4A-H3
 2.2 with sigma of 0.04
 H4A_$1-H3_$2
 2.2 with sigma of 0.04
 O4-C50 \\sim O5-C51
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O4 \\sim C50: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C50) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) = Uanis(O4)
Uanis(C51) = Uanis(C50)
5. Others
 Fixed Sof: O4(0.5) H4A(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5) O5(0.5)
 H5(0.5) C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C4(H4), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C20(H20), C21(H21), C22(H22),
  C23(H23), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48)
6.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C)
6.c Idealised tetrahedral OH refined as rotating group:
 O4(H4A), O5(H5)
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_olex2_submission_special_instructions 'No special instructions were received'