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_4315076
_publ_contact_author_address
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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         'Mo2 Cl16 C25 O10 H3, 3 (C8 H20 N)'
_chemical_formula_sum            'C49 H63 Cl16 Mo2 N3 O10'
_chemical_formula_weight         1613.10
_chemical_name_common            (NEt4)3[Mo2(Cl4C6O2)4(OCH3)(O)]
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 98.9830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4671(5)
_cell_length_b                   13.1459(5)
_cell_length_c                   19.7961(8)
_cell_measurement_reflns_used    3216
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.658
_cell_measurement_theta_min      2.878
_cell_volume                     3204.6(2)
_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      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measurement_device_type  'Bruker Smart CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15706
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  0.670
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       prism
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.59(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.016
_refine_ls_goodness_of_fit_obs   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         8503
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_restrained_S_obs      1.049
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_obs          0.0596
_refine_ls_shift/esd_max         0.190
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+9.5700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1454
_refine_ls_wR_factor_obs         0.1352
_reflns_number_gt                7007
_reflns_number_total             8503
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902328m_si_001_1.cif
_cod_data_source_block           (NEt4)3[Mo2(Cl4C6O2)4(OCH3)(O)]
_cod_depositor_comments
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The following automatic conversions were performed:
'_reflns_observed_expression' tag replaced with
'_reflns_threshold_expression' tag as specified in the replacement
file 'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 3137 2015-03-23 15:08:43Z antanas 
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_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4315076