Mononuclear Bis(dithiolene) Mo(IV) and W(IV) Complexes with P, P; S, S; O, S and O, O Donor Ligands: A Comparative Reactivity Study
Khatua, Suman; Naskar, Tilak; Nandi, Chandan; Majumdar, Amit; New J. Chem. 41 (2017) 9769–9783; doi:10.1039/C7NJ01797A

data_7056483
_publ_section_title
;
 Mononuclear Bis(dithiolene) Mo(IV) and W(IV) Complexes with P, P; S, S;
 O, S and O, O Donor Ligands: A Comparative Reactivity Study
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_journal_issue                   18
_journal_name_full               'New J. Chem.'
_journal_page_first              9769
_journal_page_last               9783
_journal_paper_doi               10.1039/C7NJ01797A
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C14 H4 N4 O S5 W, 2(C24 H20 P)'
_chemical_formula_sum            'C62 H44 N4 O P2 S5 W'
_chemical_formula_weight         1267.10
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_date             2016-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
;
_audit_update_record
;
2017-03-16 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                76.159(13)
_cell_angle_beta                 66.478(7)
_cell_angle_gamma                63.077(7)
_cell_formula_units_Z            2
_cell_length_a                   13.598(4)
_cell_length_b                   14.966(6)
_cell_length_c                   17.006(7)
_cell_measurement_reflns_used    1476
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.61
_cell_measurement_theta_min      2.54
_cell_volume                     2822.1(18)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.7-1 (Bruker-Axs,2014)'
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1431
_diffrn_reflns_av_unetI/netI     0.1917
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28764
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.862
_diffrn_reflns_theta_min         1.309
_diffrn_source_type              'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.334
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1002 before and 0.0673 after correction.
The Ratio of minimum to maximum transmission is 0.7368.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.333
_refine_diff_density_min         -2.452
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         10694
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.2080
_refine_ls_R_factor_gt           0.0947
_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^)+(0.1293P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2125
_refine_ls_wR_factor_ref         0.2751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4738
_reflns_number_total             10694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01797a2.cif
_cod_data_source_block           Wmercaptophenolate
_cod_original_cell_volume        2822.2(19)
_cod_database_code               7056483
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.736
_shelx_estimated_absorpt_t_min   0.604
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 S5A-C9 = S5B-C14
 1.68 with sigma of 0.02
 S5A-C9 = S5B-C14
 1.7 with sigma of 0.02
 O1A-C14 \\sim O1B-C9
 with sigma of 0.02
 S5A-C9 \\sim S5B-C14
 with sigma of 0.02
 W1-O1B \\sim W1-O1A
 with sigma of 0.02
 W1-S5A \\sim W1-S5B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(W1) = Uanis(S5A) = Uanis(O1B) = Uanis(S5B) = Uanis(O1A) = Uanis(C9) =
Uanis(C14) = Uanis(C13) = Uanis(C12) = Uanis(C11) = Uanis(C10)
Uanis(C27) = Uanis(C32) = Uanis(C31) = Uanis(C30) = Uanis(C29) = Uanis(C28)
Uanis(C51) = Uanis(C56) = Uanis(C55) = Uanis(C54) = Uanis(C53) = Uanis(C52)
4. Others
 Sof(S5B)=Sof(O1B)=1-FVAR(1)
 Sof(S5A)=Sof(O1A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C11(H11), C10(H10), C40(H40), C41(H41), C42(H42),
 C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52),
  C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60),
 C61(H61), C62(H62), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
5.b Fitted hexagon refined as free rotating group:
 C14(C13,C12,C11,C10,C9)
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_shelx_res_checksum              87265
_olex2_submission_special_instructions 'No special instructions were received'