A series of tetraazalene radical-bridged M2(M = CrIII, MnII, FeII, CoII) complexes with strong magnetic exchange coupling
DeGayner, Jordan A.; Jeon, Ie-Rang; Harris, T. David; Chem. Sci. 6 (2015) 6639–; doi:10.1039/C5SC02725J

data_1529409
_publ_section_title
;
 A series of tetraazalene radical-bridged M2(M = CrIII, MnII, FeII, CoII)
 complexes with strong magnetic exchange coupling
;
_journal_issue                   11
_journal_name_full               'Chem. Sci.'
_journal_page_first              6639
_journal_paper_doi               10.1039/C5SC02725J
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety
'C70 H66 Fe2 N12, 2(C32 H12 B F24), 1.5(C4 H8 O)'
_chemical_formula_sum            'C140 H102 B2 F48 Fe2 N12 O1.5'
_chemical_formula_weight         3021.65
_chemical_name_systematic        '[(TPyA)2 Fe2 (NMePh)L(2-)] 2BArF 2THF'
_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     direct
_audit_creation_date             2015-08-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-14 deposited with the CCDC.
2015-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                75.334(2)
_cell_angle_beta                 66.781(2)
_cell_angle_gamma                68.243(2)
_cell_formula_units_Z            1
_cell_length_a                   15.1719(10)
_cell_length_b                   15.9218(10)
_cell_length_c                   18.3985(12)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      67.90
_cell_measurement_theta_min      3.01
_cell_volume                     3763.5(4)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26962
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.084
_diffrn_reflns_theta_min         2.634
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.529
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0820 before and 0.0337 after correction.
The Ratio of minimum to maximum transmission is 0.8072.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dull brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       plate
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.411
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1068
_refine_ls_number_reflns         12487
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.081
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1125P)^2^+3.4404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.1864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11547
_reflns_number_total             12487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02725j2.cif
_cod_data_source_block           thismustbetheone
_cod_depositor_comments
'Adding full bibliography for 1529407--1529411.cif.'
_cod_original_formula_sum        'C140 H102 B2 F48 Fe2 N12 O1.50'
_cod_database_code               1529409
_shelxl_version_number           2014-3
_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
 C28A-C26A \\sim C35A-C28A \\sim C35A-C24A \\sim C24A-C23A \\sim C30A-C23A
\\sim C30A-C26A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C35A) \\sim Ueq, Uanis(C22A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C26A) \\sim Ueq, Uanis(C33A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C23A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C30A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26A)=Sof(C27A)=Sof(C28A)=Sof(H28A)=
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(C35A)=Sof(H35D)=1-FVAR(1)
 Sof(C22)=Sof(C23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=
 Sof(C27)=Sof(H27)=Sof(C28)=Sof(C29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=
 Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
 Fixed Sof: C5(0.75) H5A(0.75) H5B(0.75) O67(0.75) C69(0.75) H69A(0.75)
 H69B(0.75) C70(0.75) H70A(0.75) H70B(0.75) C71(0.75) H71A(0.75) H71B(0.75)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C17(H17A,H17B), C19(H19A,H19B), C5(H5A,H5B), C69(H69A,H69B),
 C70(H70A,H70B), C71(H71A,H71B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C1A(H1A), C1C(H1C), C1D(H1D), C1E(H1E), C4(H4), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C20(H20), C21(H21), C22A(H22A), C23A(H23A),
 C24(H24), C24A(H24A), C25(H25), C26(H26), C27(H27), C28A(H28A), C29A(H29A),
 C30(H30), C31(H31), C32(H32), C32A(H32A), C33(H33), C33A(H33A), C35A(H35D),
 C36(H36), C37(H37), C42(H42), C43(H43), C45(H45), C49(H49), C51(H51), C52(H52),
  C54(H54), C56(H56), C62(H62), C64(H64)
5.c Idealised Me refined as rotating group:
 C25A(H25A,H25B,H25C), C31A(H31A,H31B,H31C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C)
;
_shelx_res_checksum              82028
_olex2_submission_original_sample_id jd2-149
_olex2_submission_special_instructions 'No special instructions were received'