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_7036807
_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         'F6 Sb, C96 H88 Cr N12 O2 V2, 4(C H2 Cl2)'
_chemical_formula_sum            'C100 H96 Cl8 Cr F6 N12 O2 Sb V2'
_chemical_formula_weight         2171.11
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2015-02-12 deposited with the CCDC.
2015-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.631(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3129(7)
_cell_length_b                   22.2548(7)
_cell_length_c                   24.0941(9)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100.07
_cell_measurement_theta_max      25.750
_cell_measurement_theta_min      2.358
_cell_volume                     9869.3(6)
_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      100.07
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.998
_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  0.0837
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_laue_measured_fraction_full 0.964
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            108776
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         1.106
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
sadabs-2014/2 (Bruker,2014) was used for 
absorption correction. 
wR2(int) was 0.0916 before and 0.0606 after correction.
The Ratio of minimum to maximum transmission is 0.7444. 
The \l/2 correction factor is 0.00150.
;
_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    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             4428
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethante'
_exptl_crystal_size_max          0.716
_exptl_crystal_size_mid          0.598
_exptl_crystal_size_min          0.294
_refine_diff_density_max         1.193
_refine_diff_density_min         -1.599
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1251
_refine_ls_number_reflns         18697
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0826
_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^)+(0.0689P)^2^+99.4697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1924
_refine_ls_wR_factor_ref         0.2278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14133
_reflns_number_total             18697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02719e2.cif
_cod_data_source_block           th010_0m
_cod_depositor_comments
'Adding full bibliography for 7036804--7036807.cif.'
_cod_database_code               7036807
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.583
_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. Restrained distances
 Cl4S-Cl3S
 2.82 with sigma of 0.02
3. Others
 Sof(Sb1A)=1-FVAR(1)
 Sof(Sb1)=FVAR(1)
 Fixed Sof: Cl5S(0.66667) C3S(0.66667) H1GA(0.33333) H1GB(0.33333)
 H1GC(0.33333) H1GD(0.33333) Cl6S(0.33333) Cl6B(0.33333) Cl3S(0.33333)
 Cl4S(0.33333) C2S(0.33333) H1IA(0.33333) H1IB(0.33333)
4.a Secondary CH2 refined with riding coordinates:
 C1S(H1EA,H1EB), C5S(H1FA,H1FB), C3S(H1GA,H1GB), C3S(H1GC,H1GD), C4S(H1HA,
 H1HB), C2S(H1IA,H1IB)
4.b Aromatic/amide H refined with riding coordinates:
 C63(H5), C52(H11), C60(H15), C57(H18), C49(H1CA), C46(H22), C78(H25),
 C89(H30), C75(H34), C72(H39), C86(H42), C83(H45), C34(H58), C35(H59), C36(H60),
  C37(H61), C38(H62), C2(H67), C3(H68), C40(H70), C41(H71), C42(H72), C43(H73),
 C44(H74), C18(H75), C17(H76), C13(H77), C12(H78), C28(H80), C29(H81), C30(H82),
  C31(H83), C32(H84), C8(H85), C7(H86), C22(H88), C23(H89), C24(H90), C25(H91),
 C26(H92)
4.c Idealised Me refined as rotating group:
 C65(H1A,H1B,H1C), C54(H2A,H2B,H2C), C66(H3A,H3B,H3C), C81(H6A,H6B,H6C),
 C69(H19A,H19B,H19C), C70(H1AA,H1AB,H1AC), C55(H1BA,H1BB,H1BC), C67(H21A,H21B,
 H21C), C68(H23A,H23B,H23C), C94(H36A,H36B,H36C), C93(H38A,H38B,H38C), C92(H40A,
 H40B,H40C), C91(H41A,H41B,H41C), C95(H46A,H46B,H46C), C96(H47A,H47B,H47C),
 C80(H48A,H48B,H48C)
;
_olex2_date_sample_data_collection 2014/10/03
_olex2_date_sample_submission    2014/10/03
_olex2_submission_original_sample_id TH010
_olex2_submission_special_instructions 'No special instructions were received'