Oxido-molybdenum complexes obtained by Cl/O interchange between MoCl5 and carboxylic acids: a crystallographic, spectroscopic and computational study.
Bortoluzzi, Marco; Marchetti, Fabio; Pampaloni, Guido; Zacchini, Stefano; Dalton transactions (Cambridge, England : 2003) 43 (2014) 16416–16423; doi:10.1039/c4dt02201g

data_7032664
_publ_section_title
;
 Oxido-molybdenum complexes obtained by Cl/O interchange between MoCl5 and
 carboxylic acids: a crystallographic, spectroscopic and computational
 study.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16416
_journal_page_last               16423
_journal_paper_doi               10.1039/c4dt02201g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C4 H2 Cl12 Mo2 O6'
_chemical_formula_weight         763.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.082(3)
_cell_angle_beta                 88.495(3)
_cell_angle_gamma                75.691(3)
_cell_formula_units_Z            1
_cell_length_a                   5.9376(17)
_cell_length_b                   7.406(2)
_cell_length_c                   12.038(4)
_cell_measurement_reflns_used    3644
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      278.2455
_cell_measurement_theta_min      2.8585
_cell_volume                     509.2(3)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5458
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    2.824
_exptl_absorpt_correction_T_max  0.7281
_exptl_absorpt_correction_T_min  0.5755
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1257 (selected reflections only, before parameter refinement)
 R(int) = 0.0637 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    2.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             362
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.306
_refine_diff_density_min         -1.474
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0764P)^2^+0.4225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                2008
_reflns_number_total             2208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02201g2.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 7032663--7032664.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7032664