Molybdenum complexes with a μ-O{MoO2}2 core: their synthesis, crystal structure and application as catalysts for the oxidation of bicyclic alcohols using N-based additives
Maurya, Mannar R.; Rana, Lata; Avecilla, Fernando; New J. Chem. 41 (2017) 724–; doi:10.1039/C6NJ03162E

data_7055878
_publ_section_title
;
 Molybdenum complexes with a \m-O{MoO2}2 core: their synthesis, crystal
 structure and application as catalysts for the oxidation of bicyclic
 alcohols using N-based additives
;
_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              724
_journal_paper_doi               10.1039/C6NJ03162E
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C20 H26 Mo2 N2 O11 S2'
_chemical_formula_sum            'C20 H26 Mo2 N2 O11 S2'
_chemical_formula_weight         726.43
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-11-17 deposited with the CCDC.
2016-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.5241(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.6534(3)
_cell_length_b                   39.0383(12)
_cell_length_c                   12.9675(4)
_cell_measurement_reflns_used    114722
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      51.823
_cell_measurement_theta_min      4.429
_cell_volume                     5278.4(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            113476
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.436
_diffrn_reflns_theta_min         1.043
_exptl_absorpt_coefficient_mu    1.168
_exptl_absorpt_correction_T_max  0.7430
_exptl_absorpt_correction_T_min  0.6233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0876 before and 0.0663 after correction.
The Ratio of minimum to maximum transmission is 0.8389.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.237
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.00081(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         10802
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0350P)^2^+19.9779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9313
_reflns_number_total             10802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj03162e2.cif
_cod_data_source_block           compound3a
_cod_depositor_comments
'Adding full bibliography for 7055877--7055878.cif.'
_cod_database_code               7055878
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.724
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1A-S1B
 0.6 with sigma of 0.0001
 O8-S1A \\sim O8-S1B
 with sigma of 0.02
 S1A-C17 \\sim S1A-C18 \\sim S1B-C17 \\sim S1B-C18
 with sigma of 0.02
3. Rigid bond restraints
 S1A, S1B, O8, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
S1A \\sim S1B \\sim O8 \\sim C17 \\sim C18: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(S1B) \\sim Ueq: with sigma of 0 and sigma for terminal atoms of 0
5. Others
 Sof(S1B)=1-FVAR(1)
 Sof(S1A)=FVAR(1)
6.a Riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C23(H23), C24(H24), C25(H25), C28(H28), C29(H29), C33(H33), C34(H34), C35(H35)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C27(H27A,H27B,H27C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              65244
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'