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_1529407
_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 Cr2 N12, 4(C24 H20 B)'
_chemical_formula_sum            'C166 H146 B4 Cr2 N12'
_chemical_formula_weight         2456.18
_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                72.813(3)
_cell_angle_beta                 69.832(4)
_cell_angle_gamma                68.859(3)
_cell_formula_units_Z            1
_cell_length_a                   15.3682(7)
_cell_length_b                   15.9908(7)
_cell_length_c                   17.5923(10)
_cell_measurement_reflns_used    8107
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      68.071
_cell_measurement_theta_min      2.728
_cell_volume                     3712.1(3)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_Laue_measured_fraction_full 0.908
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23931
_diffrn_reflns_point_group_measured_fraction_full 0.908
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.073
_diffrn_reflns_theta_min         2.728
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0932 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.7910.
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    1.099
_exptl_crystal_description       plate
_exptl_crystal_F_000             1294
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.540
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         12201
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0822
_refine_ls_shift/su_max          0.064
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1578P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2053
_refine_ls_wR_factor_ref         0.2222
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8258
_reflns_number_total             12201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02725j2.cif
_cod_data_source_block           jd4_43_mcrp4
_cod_depositor_comments
'Adding full bibliography for 1529407--1529411.cif.'
_cod_database_code               1529407
_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
 C39A-C38A \\sim C38A-C36A \\sim C37A-C36A \\sim C41A-C37A \\sim C41A-C40A
\\sim C40A-C39A \\sim C46-
 C42 \\sim C52-C46 \\sim C57-C52 \\sim C57-C53 \\sim C53-C47 \\sim C47-C42
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C26A) \\sim Ueq, Uanis(C28A) \\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C31A) \\sim Ueq,
Uanis(C33A) \\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C30A) \\sim Ueq,
Uanis(C34A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C27A) \\sim Ueq,
Uanis(C35A) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(C39A) \\sim Ueq, Uanis(C38A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C40A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=
 Sof(H25B)=Sof(H25C)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(C28A)=Sof(H28A)=1-FVAR(1)
 Sof(C22)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(C32)=Sof(H32)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(H34)=FVAR(1)
 Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30A)=Sof(C31A)=Sof(H31A)=
 Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33D)=Sof(C34A)=Sof(H34A)=Sof(C35A)=1-FVAR(2)
 Sof(C23)=Sof(H23)=Sof(C24)=Sof(C25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=
 Sof(C28)=Sof(H28)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(2)
 Sof(C37A)=Sof(H37A)=Sof(C41A)=Sof(H41A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=
 Sof(H39A)=Sof(C36A)=Sof(C40A)=Sof(H40A)=1-FVAR(3)
 Sof(C54)=Sof(H54)=Sof(C48)=Sof(H48)=Sof(C59)=Sof(C49)=Sof(H49)=Sof(C55)=
 Sof(H55)=Sof(C58)=Sof(H58)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C10(H10A,H10B), C4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C15(H15), C00E(H00E), C00F(H00F), C00G(H00G), C00I(H00I), C9(H9),
 C00K(H00K), C00N(H00N), C00O(H00O), C00Q(H00Q), C00R(H00R), C00S(H00S), C8(H8),
  C00U(H00U), C00W(H00W), C00Y(H00Y), C14(H14), C13(H13), C014(H014),
 C015(H015), C7(H7), C21(H21), C12(H12), C01A(H01A), C6(H6), C01C(H01C),
 C01D(H01D), C01E(H01E), C01F(H01F), C36(H36), C18(H18), C38(H38), C23(H23),
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C44(H44), C20(H20), C32(H32),
  C57(H57), C40(H40), C51(H51), C56(H56), C50(H50), C19(H19), C46(H46),
 C47(H47), C45(H45), C52(H52), C34(H34), C53(H53), C39(H39), C43(H43), C54(H54),
  C48(H48), C49(H49), C55(H55), C58(H58), C22A(H22A), C24A(H24A), C26A(H26A),
 C28A(H28A), C31A(H31A), C32A(H32A), C33A(H33D), C34A(H34A), C37A(H37A),
 C41A(H41A), C38A(H38A), C39A(H39A), C40A(H40A)
5.c Fitted hexagon refined as free rotating group:
 C54(C48,C59,C49,C55,C58), C30A(C31A,C32A,C33A,C34A,C35A)
5.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C25A(H25A,H25B,H25C), C35(H35A,H35B,H35C), C29A(H29A,
 H29B,H29C)
;
_shelx_res_checksum              17803
_olex2_submission_special_instructions 'No special instructions were received'