Substituent Effect on Oxygen Atom Transfer Reactivity from Oxomolybdenum Centers: Synthesis, Structure, Electrochemistry, and Mechanism
Partha Basu; Victor N. Nemykin; Raghvendra S. Sengar; Inorganic Chemistry 48 (2009) 6303–6313; doi:10.1021/ic900579s

data_4302574
_publ_contact_author_address
;                                                                               
Department of Chemistry and Biochemistry
Duquesne University
Pittsburgh, PA 15282
;
_publ_contact_author_email       basu@duq.edu
_publ_contact_author_fax         '1412 396 5683'
_publ_contact_author_name        'Partha Basu'
_publ_contact_author_phone       '1412 396 6345'
_publ_section_title
;
Substituent Effect on Oxygen Atom Transfer Reactivity from Oxomolybdenum
Centers: Synthesis, Structure, Electrochemistry, and Mechanism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6303
_journal_page_last               6313
_journal_paper_doi               10.1021/ic900579s
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C22 H29 B1 Mo1 N6 O2 S1'
_chemical_formula_sum            'C22 H29 B Mo N6 O2 S'
_chemical_formula_weight         548.33
_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     direct
_audit_creation_date             09-01-25
_audit_creation_method           CRYSTALS_ver_12.85
_audit_update_record
;
2009-02-25 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 117.723(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.772(13)
_cell_length_b                   8.136(6)
_cell_length_c                   18.494(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      18
_cell_measurement_theta_min      15
_cell_volume                     2500(3)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       Unknown
_diffrn_measurement_device_type  Serial
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.094
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18392
_diffrn_reflns_theta_full        25.891
_diffrn_reflns_theta_max         26.420
_diffrn_reflns_theta_min         1.225
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.77
_refine_diff_density_min         -2.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5043
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1519
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.000184
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 13.7 16.2 6.90 2.66 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2178
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.2178
_reflns_limit_h_max              20
_reflns_limit_h_min              -23
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                1659
_reflns_number_total             5060
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.1519
_oxford_refine_ls_scale          0.2116(3)
_oxford_reflns_number_all        5043
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ic900579s_si_001_2.cif
_cod_data_source_block           Tp*MoO2(S-p-MeC6H4)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C22 H29 B1 Mo1 N6 O2 S1'
_cod_database_code               4302574