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_7056481
_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         '2(C36 H30 N P2), C14 H4 Mo N4 O S5'
_chemical_formula_sum            'C86 H64 Mo N6 O P4 S5'
_chemical_formula_weight         1577.55
_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                109.721(6)
_cell_angle_beta                 90.165(7)
_cell_angle_gamma                90.075(6)
_cell_formula_units_Z            2
_cell_length_a                   10.404(3)
_cell_length_b                   18.184(5)
_cell_length_c                   22.548(6)
_cell_measurement_reflns_used    6534
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.75
_cell_measurement_theta_min      2.29
_cell_volume                     4015.5(19)
_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 0.996
_diffrn_measured_fraction_theta_max 0.964
_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  0.0873
_diffrn_reflns_av_unetI/netI     0.1148
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            41022
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.681
_diffrn_reflns_theta_min         0.959
_diffrn_source_type              'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1666 before and 0.0681 after correction.
The Ratio of minimum to maximum transmission is 0.5580.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.116
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         16360
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.0687
_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^)+(0.1313P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8391
_reflns_number_total             16360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01797a2.cif
_cod_data_source_block           MoMercaptophenolate
_cod_original_cell_volume        4015.8(18)
_cod_database_code               7056481
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.898
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C13B-C12B \\sim C12B-C11B \\sim C11B-C10B \\sim C9B-C10B \\sim C9B-C14B \\sim
C14B-C13B \\sim C9A-
 C14A \\sim C9A-C10A \\sim C11A-C10A \\sim C12A-C11A \\sim C13A-C12A \\sim
C14A-C13A
 with sigma of 0.02
 O1A-C9A \\sim O1B-C14B
 with sigma of 0.02
 S5B-C9B \\sim S5A-C14A
 with sigma of 0.02
 Mo1-S5B \\sim Mo1-S5A
 with sigma of 0.02
 Mo1-O1A \\sim Mo1-O1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1A) = Uanis(S5B)
Uanis(O1B) = Uanis(S5A)
Uanis(C10A) = Uanis(C11A) = Uanis(C12A) = Uanis(C13A) = Uanis(C14A) = Uanis(C9A)
Uanis(C14B) = Uanis(C9B) = Uanis(C10B) = Uanis(C11B) = Uanis(C12B) = Uanis(C13B)
4. Others
 Sof(O1B)=Sof(S5B)=1-FVAR(1)
 Sof(O1A)=Sof(S5A)=FVAR(1)
 Sof(C9B)=Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(H11B)=Sof(C12B)=Sof(H12B)=
 Sof(C13B)=Sof(H13B)=Sof(C14B)=1-FVAR(2)
 Sof(C9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=
 Sof(C13A)=Sof(H13A)=Sof(C14A)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 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), 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), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68),
  C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C76(H76), C77(H77),
 C78(H78), C79(H79), C80(H80), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86),
  C10A(H10A), C10B(H10B), C11A(H11A), C11B(H11B), C12A(H12A), C12B(H12B),
 C13A(H13A), C13B(H13B)
;
_shelx_res_checksum              19905
_olex2_submission_special_instructions 'No special instructions were received'