Molybdenum(vi) tris(amidophenoxide) complexes.
Erickson, Alexander N.; Brown, Seth N.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15583–15595; doi:10.1039/c8dt03392g

data_7047781
_publ_section_title
;
 Molybdenum(vi) tris(amidophenoxide) complexes.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15583
_journal_page_last               15595
_journal_paper_doi               10.1039/c8dt03392g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C80 H102 Mo2 N4 O7, C7 D8'
_chemical_formula_sum            'C87 H102 D8 Mo2 N4 O7'
_chemical_formula_weight         1523.71
_chemical_name_common            '/m(O)-(Mo(O)(^H^ap)(^H^apH))~2~ . C7D8'
_chemical_name_systematic
'\m-oxo-bis(oxo-(2-(phenylamido)-4,6-di-tert-butylphenoxo)- (2-(phenylamino)-4,6-di-tert-butylphenoxo)molybdenum(VI))deuterotoluene solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-08-15 deposited with the CCDC.
2018-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.0155(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4155(8)
_cell_length_b                   23.0354(11)
_cell_length_c                   22.6673(11)
_cell_measurement_reflns_used    9321
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.56
_cell_volume                     8103.6(7)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa X8-APEX-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            154868
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.149
_diffrn_reflns_theta_min         1.298
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
L. Krause, R. Herbst-Irmer, G. M. Sheldrick & D. Stalke. J. Appl.
Cryst., 2015, 48, 3.
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             3200
_exptl_crystal_recrystallization_method
'The ligand ^H^apH~2~ was reacted with MoO~2~(acac)~2~ in Toluene-d~8~. Toluene was removed in vacuo and the residue was dissolved in hexanes. Crystals deposited on standing 3 months at room temperature.'
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1310
_refine_ls_number_reflns         19803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+7.0062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16394
_reflns_number_total             19803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03392g2.cif
_cod_data_source_block           moac3
_cod_depositor_comments
'Adding full bibliography for 7047780--7047786.cif.'
_cod_database_code               7047781
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.874
_shelx_estimated_absorpt_t_max   0.943
_shelx_res_checksum              25534