A general synthesis approach in action: preparation and characterization of polyoxomolybdenum(vi) organophosphonates through oxidative Mo‒Mo bond cleavage in {MoV2O4}
Zhang, Lijuan; Sun, Jingmei; Zhou, Yunshan; ul Hassan, Sadaf; Wang, Enbo; Shi, Zonghai; CrystEngComm 14 (2012) 4826–; doi:10.1039/c2ce25093d

data_7208068
_publ_section_title
;
 A general synthesis approach in action: preparation and characterization
 of polyoxomolybdenum(vi) organophosphonates through oxidative Mo--Mo bond
 cleavage in {MoV2O4}
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              4826
_journal_paper_doi               10.1039/c2ce25093d
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C4 H54 Fe Mo4 N7 O36 P4'
_chemical_formula_weight         1340.03
_chemical_name_systematic
;

?

;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n 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            2
_cell_length_a                   9.0500(3)
_cell_length_b                   19.4931(7)
_cell_length_c                   12.0533(4)
_cell_measurement_reflns_used    1273
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.76
_cell_measurement_theta_min      2.48
_cell_volume                     2126.35(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1969
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    1.742
_exptl_absorpt_correction_T_max  0.9027
_exptl_absorpt_correction_T_min  0.7926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1338
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         1.483
_refine_diff_density_min         -2.179
_refine_diff_density_rms         0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1969
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+72.1922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.1989
_reflns_number_gt                1578
_reflns_number_total             1969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25093d.txt
_cod_data_source_block           100531d_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      Pnnm
_cod_database_code               7208068