Oxidomolybdenum complexes for acid catalysis using alcohols as solvents and reactants
Gomes, Ana C.; Neves, Patrícia; Cunha-Silva, Luís; Valente, Anabela A.; Gonçalves, Isabel S.; Pillinger, Martyn; Catalysis Science & Technology 6 (2016) 5207–; doi:10.1039/C5CY02052B

data_1553093
_publ_section_title
;
 Oxidomolybdenum complexes for acid catalysis using alcohols as solvents
 and reactants
;
_journal_issue                   13
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              5207
_journal_paper_doi               10.1039/C5CY02052B
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C36 H48 Cl2 Mo2 N4 O4, 5(C H Cl3)'
_chemical_formula_sum            'C41 H53 Cl17 Mo2 N4 O4'
_chemical_formula_weight         1460.40
_space_group_crystal_system      cubic
_space_group_IT_number           228
_space_group_name_Hall           '-F 4ud 2vw 3'
_space_group_name_H-M_alt        'F d -3 c :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             '21 October 2015'
_audit_creation_method           'SHELXL-2014/7 and enCIFer'
_audit_update_record
;
2015-11-09 deposited with the CCDC.
2016-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            96
_cell_length_a                   58.3972(4)
_cell_length_b                   58.3972(4)
_cell_length_c                   58.3972(4)
_cell_measurement_reflns_used    3524
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.76
_cell_measurement_theta_min      2.42
_cell_volume                     199148(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1231
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       69
_diffrn_reflns_limit_h_min       -67
_diffrn_reflns_limit_k_max       61
_diffrn_reflns_limit_k_min       -69
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            302253
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         3.742
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'SADABS V2012/1 (Bruker AXS Inc.)' 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       prism
_exptl_crystal_F_000             70272
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         7298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0880P)^2^+2425.5254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5343
_reflns_number_total             7298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cy02052b2.cif
_cod_data_source_block           comp4CHCl3-ig0312
_cod_original_cell_volume        199148(4)
_cod_original_sg_symbol_Hall     '-F 4cvw 2vw 3'
_cod_original_sg_symbol_H-M      'F d -3 c'
_cod_database_code               1553093
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.851
_shelx_estimated_absorpt_t_max   0.872
_shelx_res_checksum              89234