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_1540626
_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_absolute_configuration ad
_chemical_formula_moiety         'C54 H78 Mo N2 O2'
_chemical_formula_sum            'C54 H78 Mo N2 O2'
_chemical_formula_weight         883.12
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                74.5019(14)
_cell_angle_beta                 87.3130(14)
_cell_angle_gamma                78.6415(14)
_cell_formula_units_Z            1
_cell_length_a                   10.0435(8)
_cell_length_b                   10.3143(8)
_cell_length_c                   12.8862(11)
_cell_measurement_reflns_used    9719
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      2.21
_cell_volume                     1261.15(18)
_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 0.985
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6861
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_laue_measured_fraction_full 0.985
_diffrn_reflns_laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13007
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        24.309
_diffrn_reflns_theta_max         29.356
_diffrn_reflns_theta_min         1.997
_diffrn_source                   'Daresbury SRS station 9.8'
_diffrn_standards_decay_%        17
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03, Sheldrick, G.M., (2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         11751
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0373P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         1.000
_reflns_friedel_fraction_full    0.985
_reflns_friedel_fraction_max     0.890
_reflns_number_gt                11618
_reflns_number_total             11751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            catalysts-05-00-1928-CIF.cif
_cod_data_source_block           1
_cod_database_code               1540626
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.960
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              51530
_shelx_hkl_checksum              72085