Behavior of anionic molybdenum(iv, vi) and tungsten(iv, vi) complexes containing bulky hydrophobic dithiolate ligands and intramolecular NHS hydrogen bonds in nonpolar solvents.
Hasenaka, Yuki; Okamura, Taka-Aki; Tatsumi, Miki; Inazumi, Naoya; Onitsuka, Kiyotaka; Dalton transactions (Cambridge, England : 2003) 43 (2014) 15491–15502; doi:10.1039/c4dt01646g

data_7032147
_publ_section_title
;
 Behavior of anionic molybdenum(iv, vi) and tungsten(iv, vi) complexes
 containing bulky hydrophobic dithiolate ligands and intramolecular NHS
 hydrogen bonds in nonpolar solvents.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15491
_journal_page_last               15502
_journal_paper_doi               10.1039/c4dt01646g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C166 H219 N11 O6 S4 W'
_chemical_formula_sum            'C166 H219 N11 O6 S4 W'
_chemical_formula_weight         2776.60
_chemical_name_systematic
;
(NEt4)2[WO2{S2C6H2[NHCOC(C6H4-t-Bu)3]2}2]-5(CH3CN) 
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Efflorescent'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           34
_space_group_name_Hall           'P 2 -2n'
_space_group_name_H-M_alt        'P n n 2'
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-08-0
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.503(2)
_cell_length_b                   25.170(5)
_cell_length_c                   21.806(4)
_cell_measurement_reflns_used    27667
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.06
_cell_volume                     7960(2)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.1065
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39616
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.069
_diffrn_source
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.9213
_exptl_absorpt_correction_T_min  0.8510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            reddish-orange
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2956
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.232
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.37(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         13726
_refine_ls_number_restraints     603
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1767
_refine_ls_R_factor_gt           0.1164
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1777P)^2^+15.4038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3046
_refine_ls_wR_factor_ref         0.3496
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                7609
_reflns_number_total             13726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01646g2.cif
_cod_data_source_block           2-W-5(CH3CN)
_cod_depositor_comments
'Adding full bibliography for 7032142--7032147.cif.'
_cod_original_cell_volume        7960(3)
_cod_database_code               7032147
_shelx_estimated_absorpt_t_min   0.851
_shelx_estimated_absorpt_t_max   0.921
_shelxl_version_number           2014/6