Deoxydehydration of Polyols Catalyzed by a Molybdenum Di-oxo-Complex Supported by a Dianionic ONO Pincer Ligand.
Tran, Randy; Kilyanek, Stefan M.; Dalton Transactions  (2019) –; doi:10.1039/C9DT03759D

data_7701335
_publ_section_title
;
 Deoxydehydration of Polyols Catalyzed by a Molybdenum Di-oxo-Complex
 Supported by a Dianionic ONO Pincer Ligand.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03759D
_journal_year                    2019
_chemical_formula_moiety         'C51 H58 Mo N O5 P'
_chemical_formula_sum            'C51 H58 Mo N O5 P'
_chemical_formula_weight         891.89
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-12-22 deposited with the CCDC.    2019-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                97.5508(10)
_cell_angle_beta                 105.1882(8)
_cell_angle_gamma                102.4915(8)
_cell_formula_units_Z            2
_cell_length_a                   9.9185(2)
_cell_length_b                   14.9484(4)
_cell_length_c                   16.3217(4)
_cell_measurement_reflns_used    9717
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.64
_cell_volume                     2234.25(9)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_molecular_graphics    'Mercury (CCDC, 2018)'
_computing_publication_material  'SHELXL-2018/1 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Photon II cpad'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            77479
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.061
_diffrn_reflns_theta_min         2.290
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  0.6042
_exptl_absorpt_correction_T_min  0.5191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       rod
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         13083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11584
_reflns_number_total             13083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03759d2.cif
_cod_data_source_block           18279
_cod_database_code               7701335
_shelx_estimated_absorpt_t_min   0.905
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              20328