Sorting the Assemblies of Unsymmetrically Covalently Functionalized Mn-Anderson Polyoxometalate Clusters with Mass Spectrometry
Yu-Fei Song; De-Liang Long; Stephanie E. Kelly; Leroy Cronin; Inorganic Chemistry 47 (2008) 9137–9139; doi:10.1021/ic801366r

data_4306548
_publ_section_title
;
Sorting the Assemblies of Unsymmetrically Covalently Functionalized
Mn-Anderson Polyoxometalate Clusters with Mass Spectrometry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9137
_journal_page_last               9139
_journal_paper_doi               10.1021/ic801366r
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C66 H135 Mn Mo6 N6 O27'
_chemical_formula_weight         2075.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.939(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.8017(19)
_cell_length_b                   13.6385(12)
_cell_length_c                   26.880(2)
_cell_measurement_reflns_used    4582
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.41
_cell_measurement_theta_min      2.24
_cell_volume                     9070.9(13)
_computing_cell_refinement       'Apex 2'
_computing_data_collection       'Apex 2'
_computing_data_reduction        'Apex 2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.748
_diffrn_measured_fraction_theta_max 0.748
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       '\w & \p 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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.1020
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28395
_diffrn_reflns_theta_full        23.33
_diffrn_reflns_theta_max         23.33
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  0.8886
_exptl_absorpt_correction_T_min  0.7796
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4264
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.48
_refine_diff_density_min         -0.74
_refine_diff_density_rms         0.18
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         9841
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1997
_refine_ls_R_factor_gt           0.1092
_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^)+(0.1292P)^2^+228.4506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2666
_refine_ls_wR_factor_ref         0.3538
_reflns_number_gt                4939
_reflns_number_total             9841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801366r_si_001_2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        9071.0(13)
_cod_database_code               4306548