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_7055877
_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         'C36 H56 Mo2 N4 O9, 3(C3 H7 N O)'
_chemical_formula_sum            'C45 H77 Mo2 N7 O12'
_chemical_formula_weight         1100.01
_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_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-11-17
_audit_creation_method
;
 Olex2 1.2
 (compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2016-11-17 deposited with the CCDC.
2016-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                79.12(2)
_cell_angle_beta                 74.44(2)
_cell_angle_gamma                77.50(2)
_cell_formula_units_Z            2
_cell_length_a                   10.510(5)
_cell_length_b                   15.733(7)
_cell_length_c                   18.670(8)
_cell_measurement_reflns_used    39012
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      56.293
_cell_measurement_theta_min      4.476
_cell_volume                     2875(2)
_computing_molecular_graphics
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37100
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.456
_diffrn_reflns_theta_min         1.339
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.9521
_exptl_absorpt_correction_T_min  0.8654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_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    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.669
_refine_diff_density_min         -1.753
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         13556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0584
_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^)+(0.1633P)^2^+5.7082P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.2634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9719
_reflns_number_total             13556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj03162e2.cif
_cod_data_source_block           compound1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7055877--7055878.cif.
;
_cod_original_sg_symbol_Hall     'P 1'
_cod_original_sg_symbol_H-M      'P 1'
_cod_database_code               7055877
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.866
_shelx_fab_checksum              42192
_shelx_res_checksum              69618
_reflns_friedel_fraction
;
 is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_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.a Riding coordinates:
 C1D(H1D), C4D(H4D), C10D(H10D), C13D(H13D)
 2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7D(H7D), C15(H15), C16(H16), C18(H18), C20(H20)
 2.c Idealised Me refined as rotating group:
 C2D(H2DA,H2DB,H2DC), C3D(H3DA,H3DB,H3DC), C5D(H5DA,H5DB,H5DC), C6D(H6DA,H6DB,
 H6DC), C8(H8A,H8B,H8C), C8D(H8DA,H8DB,H8DC), C9(H9A,H9B,H9C), C9D(H9DA,H9DB,
 H9DC), C10(H10A,H10B,H10C), C11D(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C12D(H12D,H12E,H12F), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C14D(H14D,H14E,
 H14F), C15D(H15A,H15B,H15C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C),
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_olex2_submission_special_instructions 'No special instructions were received'