Molybdenum (VI) Imido Complexes Derived from Chelating Phenols: Synthesis, Characterization and ɛ-Caprolactone ROP Capability
Al-Khafaji, Yahya; Prior, Timothy; Elsegood, Mark; Redshaw, Carl; Catalysts 5 (2015) 1928–; doi:10.3390/catal5041928

data_1540629
_publ_section_title
;
 Molybdenum (VI) Imido Complexes Derived from Chelating Phenols:
 Synthesis, Characterization and &#x025B;-Caprolactone ROP Capability
;
_journal_issue                   4
_journal_name_full               Catalysts
_journal_page_first              1928
_journal_paper_doi               10.3390/catal5041928
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C102 H140 Mo2 N4 O8, 6(C2 H3 N)'
_chemical_formula_sum            'C114 H158 Mo2 N10 O8'
_chemical_formula_weight         1988.37
_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   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                106.1133(10)
_cell_angle_beta                 96.4972(10)
_cell_angle_gamma                92.7062(10)
_cell_formula_units_Z            1
_cell_length_a                   13.0178(8)
_cell_length_b                   13.4853(8)
_cell_length_c                   16.9177(10)
_cell_measurement_reflns_used    8829
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.29
_cell_volume                     2825.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.867
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25167
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.028
_diffrn_reflns_theta_min         1.577
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03, Sheldrick, G.M., (2001)'
_exptl_crystal_colour            'Dark orange'
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         13076
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0425P)^2^+1.8421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10128
_reflns_number_total             13076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            catalysts-05-00-1928-CIF.cif
_cod_data_source_block           4-6MeCN
_cod_database_code               1540629
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              12027
_shelx_hkl_checksum              83209