Metal and Ligand Effects on Bonding in Group 6 Complexes of Redox-Active Amidodiphenoxides
Ranis, Leila G.; Werellapatha, Kalpani; Pietrini, Nicholas J.; Bunker, Bruce A.; Brown, Seth N.; Inorganic Chemistry  (2014) 140923084651005–; doi:10.1021/ic501222n

data_4341126
_publ_section_title
;
 Metal and Ligand Effects on Bonding in Group 6 Complexes of Redox-Active
 Amidodiphenoxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              140923084651005
_journal_paper_doi               10.1021/ic501222n
_journal_year                    2014
_chemical_formula_moiety         'C56 H76 Mo N2 O6'
_chemical_formula_sum            'C56 H76 Mo N2 O6'
_chemical_formula_weight         969.13
_chemical_name_common            (DOPO)2Mo
_chemical_name_systematic
; 
 Bis(2,4,6,8-tetra-tert-butyl-1,9-dioxophenoxazinato)molybdenum(VI) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     isomor
_atom_sites_solution_secondary   none
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.849(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.518(2)
_cell_length_b                   19.860(2)
_cell_length_c                   12.9284(14)
_cell_measurement_reflns_used    5301
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.58
_cell_volume                     5267.6(9)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'XL (Sheldrick, 2001)'
_computing_structure_solution    'XS (Sheldrick, 2001)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1257
_diffrn_reflns_av_sigmaI/netI    0.1416
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38852
_diffrn_reflns_theta_full        26.53
_diffrn_reflns_theta_max         26.53
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  0.9870
_exptl_absorpt_correction_T_min  0.9354
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Blessing, R. H. (1995) Acta Cryst. A51, 33-38.

Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. 
Madison, WI USA.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'blocky fragment'
_exptl_crystal_F_000             2064
_exptl_crystal_recrystallization_method
;
 Vapor diffusion of acetonitrile into CDCl3.
;
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.778
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         10868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                6426
_reflns_number_total             10868
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501222n_si_003.cif
_cod_data_source_block           modopo
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        5267.5(10)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4341126