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_1529411
_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         '2(C70 H66 Cr2 N12), 6(C24 H20 B), 4(C2 H3 N)'
_chemical_formula_sum            'C292 H264 B6 Cr4 N28'
_chemical_formula_weight         4438.16
_chemical_name_systematic        '[(TPyA)2 Cr2 (NMePh)L(3-)] 3(BPh4) 2(CH3CN)'
_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             2015-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-22 deposited with the CCDC.
2015-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.924(2)
_cell_angle_beta                 97.350(2)
_cell_angle_gamma                115.288(2)
_cell_formula_units_Z            1
_cell_length_a                   15.1700(6)
_cell_length_b                   15.9112(6)
_cell_length_c                   30.3415(11)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.49
_cell_measurement_theta_min      3.08
_cell_volume                     6546.9(4)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.846
_diffrn_measured_fraction_theta_max 0.958
_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  0.0708
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.846
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41642
_diffrn_reflns_point_group_measured_fraction_full 0.846
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.555
_diffrn_reflns_theta_min         1.473
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.783
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.6209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0856 before and 0.0543 after correction.
The Ratio of minimum to maximum transmission is 0.8254.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_description       plate
_exptl_crystal_F_000             2338
_exptl_crystal_size_max          0.699
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1728
_refine_ls_number_reflns         20036
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0812
_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^)+(0.1620P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2147
_refine_ls_wR_factor_ref         0.2395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13435
_reflns_number_total             20036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02725j2.cif
_cod_data_source_block           jd4_27_mcrp
_cod_depositor_comments
'Adding full bibliography for 1529407--1529411.cif.'
_cod_database_code               1529411
_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. Uiso/Uaniso restraints and constraints
Uanis(C25A) \\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C27A) \\sim Ueq,
Uanis(C32A) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C28A) \\sim Ueq, Uanis(C84A)
\\sim Ueq, Uanis(C66A) \\sim Ueq, Uanis(C68A) \\sim Ueq, Uanis(C77A) \\sim Ueq,
Uanis(C26A) \\sim Ueq, Uanis(C76A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C30A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3. Others
 Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23A)=Sof(C24A)=Sof(H24A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=1-FVAR(1)
 Sof(C22)=Sof(C23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=
 Sof(C27)=Sof(H27)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30A)=Sof(C31A)=Sof(C32A)=
 Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34D)=Sof(C35A)=Sof(H35D)=1-FVAR(2)
 Sof(C28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=
 Sof(H32)=Sof(C33)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(2)
 Sof(C72A)=Sof(H72A)=Sof(C74A)=Sof(H74A)=Sof(C76A)=Sof(C77A)=Sof(C78A)=
 Sof(H78A)=Sof(C70A)=Sof(H70A)=Sof(C80A)=Sof(H80A)=Sof(H80B)=Sof(H80C)=1-FVAR(3)
 Sof(C60)=Sof(C65)=Sof(H65)=Sof(C68)=Sof(H68)=Sof(C72)=Sof(C77)=Sof(H77A)=
 Sof(H77B)=Sof(H77C)=Sof(C81)=Sof(H81)=Sof(C83)=Sof(H83)=FVAR(3)
 Sof(C57A)=Sof(H57A)=Sof(C59A)=Sof(C60A)=Sof(H60A)=Sof(H60B)=Sof(H60C)=
 Sof(C64A)=Sof(H64A)=Sof(C66A)=Sof(H66A)=Sof(C68A)=Sof(H68A)=Sof(C84A)=1-FVAR(4)
 Sof(C57)=Sof(C58)=Sof(H58)=Sof(C61)=Sof(H61)=Sof(C63)=Sof(H63)=Sof(C67)=
 Sof(C70)=Sof(H70)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=FVAR(4)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C4(H4A,H4B), C39(H39A,H39B), C45(H45A,H45B), C51(H51A,H51B),
 C1F(H1FA,H1FB)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C9(H9), C00M(H00M), C00O(H00O), C00P(H00P), C00Q(H00Q), C15(H15),
 C00Z(H00Z), C36(H36), C012(H012), C014(H014), C015(H015), C017(H017),
 C018(H018), C01A(H01A), C01B(H01B), C6(H6), C41(H41), C01F(H01F), C42(H42),
 C01H(H01H), C7(H7), C01K(H01K), C13(H13), C8(H8), C14(H14), C24(H24), C25(H25),
  C26(H26), C27(H27), C01Q(H01Q), C01R(H01R), C1A(H1A), C12(H12), C01V(H01V),
 C01X(H01X), C01Y(H01Y), C01Z(H01Z), C020(H020), C021(H021), C022(H022),
 C023(H023), C024(H024), C025(H025), C026(H026), C43(H43), C029(H029), C50(H50),
  C02B(H02B), C47(H47), C02G(H02G), C02H(H02H), C02I(H02I), C02K(H02K),
 C02L(H02L), C02M(H02M), C21(H21), C02O(H02O), C02P(H02P), C02R(H02R),
 C02S(H02S), C02T(H02T), C02U(H02U), C02W(H02W), C02X(H02X), C02Z(H02Z),
 C030(H030), C58(H58), C49(H49), C48(H48), C036(H036), C56(H56), C18(H18),
 C03A(H03A), C03D(H03D), C03E(H03E), C03G(H03G), C61(H61), C03I(H03I), C63(H63),
  C29(H29), C30(H30), C31(H31), C32(H32), C03M(H03M), C19(H19), C03O(H03O),
 C03P(H03P), C20(H20), C03R(H03R), C03T(H03T), C03U(H03U), C53(H53), C03X(H03X),
  C55(H55), C65(H65), C54(H54), C044(H044), C68(H68), C70(H70), C81(H81),
 C83(H83), C24A(H24A), C25A(H25A), C26A(H26A), C27A(H27A), C32A(H32A),
 C33A(H33A), C34A(H34D), C35A(H35D), C57A(H57A), C64A(H64A), C66A(H66A),
 C68A(H68A), C72A(H72A), C74A(H74A), C78A(H78A), C70A(H70A)
4.c Fitted hexagon refined as free rotating group:
 C23A(C24A,C25A,C26A,C27A,C28A), C72A(C74A,C76A,C77A,C78A,C70A)
4.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C73(H73A,H73B,H73C), C77(H77A,H77B,
 H77C), C04G(H04D,H04E,H04F), C04J(H04A,H04B,H04C), C22A(H22A,H22B,H22C),
 C29A(H29A,H29B,H29C), C60A(H60A,H60B,H60C), C80A(H80A,H80B,H80C)
;
_shelx_res_checksum              14917
_olex2_submission_special_instructions 'No special instructions were received'