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_1529408
_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 Mn2 N12, 2(C32 H12 B F24)'
_chemical_formula_sum            'C134 H90 B2 F48 Mn2 N12'
_chemical_formula_weight         2911.67
_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             2015-04-21
_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                75.382(2)
_cell_angle_beta                 67.031(2)
_cell_angle_gamma                68.819(2)
_cell_formula_units_Z            1
_cell_length_a                   15.0589(5)
_cell_length_b                   15.8311(5)
_cell_length_c                   18.4096(6)
_cell_measurement_reflns_used    9338
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      68.219
_cell_measurement_theta_min      5.721
_cell_volume                     3736.0(2)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_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      100.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.957
_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  0.0265
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.904
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17083
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.080
_diffrn_reflns_theta_min         5.721
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    2.339
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0604 before and 0.0370 after correction.
The Ratio of minimum to maximum transmission is 0.7500.
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    1.294
_exptl_crystal_description       plate
_exptl_crystal_F_000             1470
_exptl_crystal_size_max          0.517
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1023
_refine_ls_number_reflns         12202
_refine_ls_number_restraints     282
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1169P)^2^+1.0375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.1831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10110
_reflns_number_total             12202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02725j2.cif
_cod_data_source_block           mmnb
_cod_depositor_comments
'Adding full bibliography for 1529407--1529411.cif.'
_cod_database_code               1529408
_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
 C23-C22 \\sim C24-C23 \\sim C25-C24 \\sim C23A-C22A \\sim C26-C25 \\sim
C26A-C22A \\sim C27-C26 ~
 C31A-C26A \\sim C31A-C30A \\sim C30A-C24A \\sim C24A-C23A \\sim C27-C22 \\sim
C35A-C32A \\sim C35A-
 C27A \\sim C34A-C27A \\sim C34A-C33A \\sim C32A-C25A \\sim C29-C28 \\sim
C33A-C25A \\sim C30-C29 \\sim C31-
 C30 \\sim C32-C31 \\sim C33-C32 \\sim C33-C28
 with sigma of 0.02
 C34-C26 \\sim C28A-C24A \\sim C35-C33 \\sim C29A-C25A
 with sigma of 0.02
3. Others
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(C24A)=Sof(C25A)=Sof(C26A)=Sof(H26A)=
 Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29A)=
 Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31A)=
 Sof(C32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34D)=Sof(C35A)=Sof(H35D)=1-FVAR(1)
 Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(C26)=
 Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=
 Sof(C31)=Sof(H31)=Sof(C32)=Sof(C33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C16(H16A,H16B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14),
 C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C22A(H22A),
 C23(H23), C24(H24), C26A(H26A), C27(H27), C27A(H27A), C28(H28), C29(H29),
 C30(H30), C30A(H30A), C31(H31), C31A(H31A), C33A(H33A), C34A(H34D), C35A(H35D),
  C013(H013), C37(H37), C39(H39), C41(H41), C45(H45), C47(H47), C52(H52),
 C54(H54), C56(H56), C60(H60), C62(H62), C64(H64)
4.c Idealised Me refined as rotating group:
 C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C)
;
_shelx_res_checksum              53000
_olex2_submission_original_sample_id jd3-91_mMnB
_olex2_submission_special_instructions 'No special instructions were received'