A templated synthesis of tetranuclear polyoxoalkoxymolybdates(V). Bromo coordinated oxomolybdenum(V) clusters: known core structure with new ligands. Oxidation to the Lindquist anion
Barbara Modec; Jurij V. Brenčič; Jon Zubieta; J. Chem. Soc., Dalton Trans.  (2002) 1500–1507; doi:10.1039/b110062a

data_7011281
_publ_section_title
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 A templated synthesis of tetranuclear polyoxoalkoxymolybdates(V).
 Bromo coordinated oxomolybdenum(V) clusters: known core structure with
 new ligands. Oxidation to the Lindquist anion
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_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1500
_journal_page_last               1507
_journal_paper_doi               10.1039/b110062a
_journal_year                    2002
_chemical_formula_sum            'C20 H38 Mo6 N4 O21'
_chemical_formula_weight         1246.18
_chemical_name_systematic
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Tetramethylpyrazinium(2+) nonadecaoxohexamolybdate(VI).
tetrametyhlpyrazine.ethanol (1/1/2)
;
_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                77.6940(4)
_cell_angle_beta                 67.0360(4)
_cell_angle_gamma                67.1440(4)
_cell_formula_units_Z            1
_cell_length_a                   8.66390(10)
_cell_length_b                   10.82010(10)
_cell_length_c                   11.05740(10)
_cell_measurement_reflns_used    3997
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     877.162(16)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0134
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7765
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         3.89
_exptl_absorpt_coefficient_mu    2.168
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'yellow white'
_exptl_crystal_density_diffrn    2.359
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.0042(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.5839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0556
_reflns_number_gt                3608
_reflns_number_total             4020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110062a.txt
_cod_data_source_block           3
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.5839P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.5839P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        877.163(15)
_cod_database_code               7011281