Synthesis and Reactivity of Catecholate Complexes Containing Quadruply Bonded Metal Ions
Jason Christ; Corinne Epps; Victoria Pritchard; Derek Schmeh; Cortlandt Pierpont; Ebbe Nordlander; Inorganic Chemistry 49 (2010) 2029–2031; doi:10.1021/ic902328m

data_4315078
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of Colorado
Boulder, CO  80309-0215
;
_publ_contact_author_email       pierpont@colorado.edu
_publ_contact_author_fax         '01 303 492 5894'
_publ_contact_author_name        'Professor Cortlandt Pierpont'
_publ_contact_author_phone       '01 303 492 8420'
_publ_section_title
;
 Synthesis and Reactivity of Catecholate Complexes Containing Quadruply
 Bonded Metal Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2029
_journal_page_last               2031
_journal_paper_doi               10.1021/ic902328m
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'Mo O6 Cl8 C16 H8, C8 H20 N, C4 H8 O'
_chemical_formula_sum            'C28 H36 Cl8 Mo N O7'
_chemical_formula_weight         878.15
_chemical_name_common            (N(C2H5)4)[MoO(Cl4C6O2)2(C4H8O)](C4H8O)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2408(7)
_cell_length_b                   19.7260(15)
_cell_length_c                   19.3697(16)
_cell_measurement_reflns_used    3136
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      2.86
_cell_volume                     3530.8(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT/XPREP'
_computing_molecular_graphics    'SHELXP (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      138(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart CCD'
_diffrn_measurement_method       '\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  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33540
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    1.02
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_platon_squeeze_details
;
;
_refine_diff_density_max         4.991
_refine_diff_density_min         -1.841
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         5544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1083P)^2^+19.0640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2185
_refine_ls_wR_factor_ref         0.2262
_reflns_number_gt                4629
_reflns_number_total             5544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902328m_si_001_3.cif
_cod_data_source_block           (N(C2H5)4)[MoO(Cl4C6O2)2(C4H8O)](C4H8O)
_cod_database_code               4315078