An unusual trigonal D3 assembly composed of molybdate anions and multiply bonded dimolybdenum units
Donahue, James P.; Murillo, Carlos A.; Dalton Transactions  (2008) 1547–1551; doi:10.1039/b714814c

data_7003250
_publ_section_title
;
 An unusual trigonal D3 assembly composed of molybdate anions and
 multiply bonded dimolybdenum units
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              1547
_journal_page_last               1551
_journal_paper_doi               10.1039/b714814c
_journal_year                    2008
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
;
[[[(H3 C O C6 H4 N)2 C H]3 Mo2]3 (Mo O4)2][P F6]2 . (C H2 Cl2)2
;
_chemical_formula_structural
;
[[Mo2(DAniF)3]3(mu(3)-MoO4)2][PF6]2.2(CH2Cl2)
;
_chemical_formula_sum            'C137 H139 Cl4 F12 Mo8 N18 O26 P2'
_chemical_formula_weight         3652.92
_chemical_melting_point          ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 91.772(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.7246(14)
_cell_length_b                   18.0560(14)
_cell_length_c                   28.435(2)
_cell_measurement_reflns_used    9104
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.37
_cell_volume                     14740.8(17)
_computing_cell_refinement       'SAINT V. 6.02'
_computing_data_collection       'SMART V. 5.059'
_computing_data_reduction        'SAINT V. 6.02'
_computing_molecular_graphics    'SHELXTL V. 5.03 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Bruker SMART 1000'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51271
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.94
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             7348
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.260
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.036
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         16672
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_obs          0.0450
_refine_ls_shift/esd_max         -0.059
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+77.1929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1140
_refine_ls_wR_factor_obs         0.0994
_reflns_number_observed          12494
_reflns_number_total             16673
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b714814c.txt
_cod_data_source_block           Manuscript
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (71
time).

'_geom_angle_publ_flag' value 'N' changed to 'n' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (131
time).

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (39
times).

'_geom_bond_publ_flag' value 'N' changed to 'n' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (88 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+77.1929P] 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^)+(0.0410P)^2^+77.1929P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        14740.8(16)
_cod_database_code               7003250