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_7036806
_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         'C74 H54 Cl Cr F12 N8 O V, 6(C H2 Cl2)'
_chemical_formula_sum            'C80 H66 Cl13 Cr F12 N8 O V'
_chemical_formula_weight         1947.19
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_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             2014-11-18
_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                101.953(2)
_cell_angle_beta                 95.065(2)
_cell_angle_gamma                108.123(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1820(5)
_cell_length_b                   13.6961(6)
_cell_length_c                   27.0875(11)
_cell_measurement_reflns_used    9681
_cell_measurement_temperature    110.1
_cell_measurement_theta_max      26.452
_cell_measurement_theta_min      2.337
_cell_volume                     4485.3(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.1
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            102867
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         0.779
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0650 before and 0.0555 after correction.
The Ratio of minimum to maximum transmission is 0.8771.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       block
_exptl_crystal_F_000             1972
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.568
_exptl_crystal_size_mid          0.391
_exptl_crystal_size_min          0.274
_refine_diff_density_max         0.958
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1092
_refine_ls_number_reflns         18323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0747P)^2^+10.3385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1655
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13275
_reflns_number_total             18323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02719e2.cif
_cod_data_source_block           th008_0m_sq_s
_cod_depositor_comments
'Adding full bibliography for 7036804--7036807.cif.'
_cod_database_code               7036806
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.697
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H2SC)=Sof(H2SD)=Sof(Cl6S)=1-FVAR(1)
 Sof(Cl5S)=Sof(H2SA)=Sof(H2SB)=FVAR(1)
 Sof(H1SC)=Sof(H1SD)=Sof(Cl1S)=Sof(Cl4S)=1-FVAR(2)
 Sof(Cl3S)=Sof(Cl2S)=Sof(H1SA)=Sof(H1SB)=FVAR(2)
 Sof(H4SC)=Sof(H4SD)=Sof(Cl9S)=1-FVAR(3)
 Sof(Cl10)=Sof(H4SA)=Sof(H4SB)=FVAR(3)
3.a Secondary CH2 refined with riding coordinates:
 C4S(H4SA,H4SB), C4S(H4SC,H4SD), C5S(H5SA,H5SB), C2S(H2SA,H2SB), C2S(H2SC,
 H2SD), C3S(H3SA,H3SB), C6S(H6SA,H6SB), C1S(H1SA,H1SB), C1S(H1SC,H1SD)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C40(H40), C41(H41), C43(H43), C44(H44), C17(H17), C18(H18),
 C34(H34), C35(H35), C37(H37), C38(H38), C12(H12), C13(H13), C26(H26), C25(H25),
  C23(H23), C22(H22), C7(H7), C8(H8), C32(H32), C28(H28), C64(H64), C61(H61),
 C56(H56), C1A(H1A), C50(H50), C67(H67), C31(H31), C29(H29)
3.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C59(H59A,H59B,H59C), C69(H69A,H69B,H69C), C70(H70A,H70B,
 H70C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C58(H58A,H58B,H58C), C75(H75A,
 H75B,H75C)
;
_shelx_fab_checksum              44286
_olex2_submission_special_instructions 'No special instructions were received'