Ferromagnetic coupling in d(1)-d(3) linear oxido-bridged heterometallic complexes: ground-state models of metal-to-metal charge transfer excited states.
Huang, Tao; Wu, Xinyuan; Song, Xiao; Xu, Hao; Smirnova, Tatyana I.; Weare, Walter W.; Sommer, Roger D.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 18937–18944; doi:10.1039/c5dt02719e

data_7036805
_publ_section_title
;
 Ferromagnetic coupling in d(1)-d(3) linear oxido-bridged heterometallic
 complexes: ground-state models of metal-to-metal charge transfer excited
 states.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18937
_journal_page_last               18944
_journal_paper_doi               10.1039/c5dt02719e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C92 H80 Cr N12 O2 Ti V, F6 Sb'
_chemical_formula_sum            'C92 H80 Cr F6 N12 O2 Sb Ti V'
_chemical_formula_weight         1772.27
_chemical_name_systematic        Cr(TPP)(TiOTMTAA)(VOOMTAA)SbF6
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-10-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-02-12 deposited with the CCDC.
2015-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.861(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4365(8)
_cell_length_b                   22.6229(10)
_cell_length_c                   24.1293(10)
_cell_measurement_reflns_used    9054
_cell_measurement_temperature    110.1
_cell_measurement_theta_max      25.284
_cell_measurement_theta_min      2.438
_cell_volume                     9523.6(7)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.1
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_laue_measured_fraction_full 0.898
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            203167
_diffrn_reflns_point_group_measured_fraction_full 0.898
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.474
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0547 before and 0.0456 after correction.
The Ratio of minimum to maximum transmission is 0.8833.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       plate
_exptl_crystal_F_000             3624
_exptl_crystal_preparation       'Solvent diffusion from C5 to DCM'
_exptl_crystal_size_max          0.506
_exptl_crystal_size_mid          0.465
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.820
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1109
_refine_ls_number_reflns         16810
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0774
_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^)+(0.0587P)^2^+44.6724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1933
_refine_ls_wR_factor_ref         0.2122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12900
_reflns_number_total             16810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02719e2.cif
_cod_data_source_block           th002_0ma_sq_s
_cod_depositor_comments
'Adding full bibliography for 7036804--7036807.cif.'
_cod_database_code               7036805
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F3A-Sb1A
 1.8 with sigma of 0.02
 Sb1A-F2A
 1.8 with sigma of 0.02
 Sb1A-F4A
 1.8 with sigma of 0.02
 Sb1A-F5A
 1.8 with sigma of 0.02
 Sb1A-F6A
 1.8 with sigma of 0.02
 Sb1A-F1A
 1.8 with sigma of 0.02
 Sb1-F3
 1.8 with sigma of 0.02
 Sb1-F1
 1.8 with sigma of 0.02
 Sb1-F6
 1.8 with sigma of 0.02
 Sb1-F2
 1.8 with sigma of 0.02
 Sb1-F4
 1.8 with sigma of 0.02
3. Others
 Sof(F4A)=Sof(F2A)=Sof(Sb1A)=Sof(F1A)=Sof(F3A)=Sof(F6A)=Sof(F5A)=1-FVAR(1)
 Sof(Sb1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F1)=Sof(F6)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C85(H85), C79(H79), C82(H82), C74(H74), C68(H68), C71(H71), C12(H12),
 C13(H13), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C18(H18), C17(H17),
  C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C3(H3), C2(H2), C26(H26),
 C25(H25), C24(H24), C23(H23), C22(H22), C7(H7), C8(H8), C29(H29), C28(H28),
 C32(H32), C31(H31), C30(H30), C47(H47), C46(H46), C49(H49), C48(H48), C52(H52),
  C57(H57), C58(H58), C59(H59), C60(H60), C63(H63)
4.b Fitted hexagon refined as free rotating group:
 C56(C57,C58,C59,C60,C61)
4.c Idealised Me refined as rotating group:
 C87(H87A,H87B,H87C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C91(H91A,H91B,
 H91C), C92(H92A,H92B,H92C), C88(H88A,H88B,H88C), C65(H65A,H65B,H65C), C66(H66A,
 H66B,H66C), C55(H55A,H55B,H55C), C54(H54A,H54B,H54C), C90(H90A,H90B,H90C),
 C89(H89A,H89B,H89C)
;
_shelx_fab_checksum              42798
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_exptl_crystal_mounting_method
'Crystal was selected under proctection of dry ice and mount it quickly.'
_olex2_submission_special_instructions 'No special instructions were received'