Mono-oxo molybdenum(vi) and tungsten(vi) complexes bearing chelating aryloxides: synthesis, structure and ring opening polymerization of cyclic esters
Sun, Ziyue; Zhao, Yanxia; Prior, Timothy J.; Elsegood, Mark R. J.; Wang, Kuiyuan; Xing, Tian; Redshaw, Carl; Dalton Transactions  (2019) –; doi:10.1039/C8DT04566F

data_7048573
_publ_section_title
;
 Mono-oxo molybdenum(vi) and tungsten(vi) complexes bearing chelating
 aryloxides: synthesis, structure and ring opening polymerization of
 cyclic esters
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT04566F
_journal_year                    2019
_chemical_formula_moiety         'C60 H88 Mo O5, 2(C2 H3 N)'
_chemical_formula_sum            'C64 H94 Mo N2 O5'
_chemical_formula_weight         1067.35
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-08-10 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.387(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3081(6)
_cell_length_b                   18.8028(10)
_cell_length_c                   27.2978(13)
_cell_measurement_reflns_used    16218
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      1.3
_cell_volume                     6312.0(5)
_computing_cell_refinement       'Stoe X-AREA'
_computing_data_collection       'Stoe X-AREA'
_computing_data_reduction
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_computing_molecular_graphics    'Bruker SHELTL'
_computing_publication_material  'Bruker SHELTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0799
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            29575
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.881
_diffrn_reflns_theta_min         1.315
_diffrn_source                   'Fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.817
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         13335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.817
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0335P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8155
_reflns_number_total             13335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04566f2.cif
_cod_data_source_block           1dot2MeCN
_cod_database_code               7048573
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.935
_shelx_estimated_absorpt_t_max   0.963
_shelx_res_checksum              3818