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_1529410
_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 Co2 N12, 2(C32 H12 B F24)'
_chemical_formula_sum            'C134 H76 B2 Co2 F48 N12'
_chemical_formula_weight         2905.54
_chemical_name_systematic        '[(TPyA)2 Co2 (NMePh)L2-] 2BArF'
_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                75.560(2)
_cell_angle_beta                 67.648(2)
_cell_angle_gamma                68.820(2)
_cell_formula_units_Z            1
_cell_length_a                   14.8476(4)
_cell_length_b                   15.9017(4)
_cell_length_c                   18.2100(5)
_cell_measurement_reflns_used    6533
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      64.980
_cell_measurement_theta_min      2.646
_cell_volume                     3676.39(18)
_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      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.970
_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  0.0297
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_laue_measured_fraction_full 0.917
_diffrn_reflns_laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18375
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.121
_diffrn_reflns_theta_min         2.646
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    2.746
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0443 before and 0.0358 after correction.
The Ratio of minimum to maximum transmission is 0.9018.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dull bluish brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       plate
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1024
_refine_ls_number_reflns         12190
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0668
_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^)+(0.1117P)^2^+1.1150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1773
_refine_ls_wR_factor_ref         0.1936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8612
_reflns_number_total             12190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02725j2.cif
_cod_data_source_block           nmephco2barf
_cod_depositor_comments
'Adding full bibliography for 1529407--1529411.cif.'
_cod_original_cell_volume        3676.40(18)
_cod_database_code               1529410
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.538
_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
 C29-C34 \\sim C28A-C26A \\sim C28-C22 \\sim C29A-C30A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C28A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30A)=Sof(C31A)=Sof(C32A)=
 Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=1-FVAR(1)
 Sof(C22)=Sof(H22B)=Sof(H22C)=Sof(H22D)=Sof(C23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=FVAR(1)
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=
 Sof(H25A)=Sof(C26A)=Sof(C27A)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=1-FVAR(2)
 Sof(C29)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=
 Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(C35)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C10(H10A,H10B), C16(H16A,H16B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22A(H22A), C23A(H23A),
 C24(H24), C24A(H24A), C25(H25), C25A(H25A), C26(H26), C27(H27), C30(H30),
 C31(H31), C32(H32), C32A(H32A), C33(H33), C33A(H33A), C34A(H34A), C35A(H35A),
 C37(H37), C39(H39), C41(H41), C45(H45), C47(H47), C49(H49), C54(H54), C56(H56),
  C58(H58), C62(H62), C64(H64), C66(H66)
5.c Idealised Me refined as rotating group:
 C22(H22B,H22C,H22D), C28A(H28A,H28B,H28C), C29(H29D,H29E,H29F), C29A(H29A,
 H29B,H29C)
;
_shelx_res_checksum              47729
_olex2_submission_original_sample_id 'jd2-99a mCoB'
_olex2_submission_special_instructions 'No special instructions were received'