Polyoxometalate-Diphosphate Complexes. 5.1 Cigar-Shaped 30-Molybdobispyrophosphate: Structure of (N(C4H9)4)2H9[{(P2O7)Mo15O45}2][PMo12O40]
Ulrich Kortz; Inorganic Chemistry 39 (2000) 623–624; doi:10.1021/ic9907258

data_4300074
_publ_contact_author_address
;
Department of Chemistry
American University of Beirut
Bliss street, POB 11-0236
Beirut, LEBANON
;
_publ_contact_author_email
;
ulrich.kortz@aub.edu.lb
;
_publ_contact_author_fax
;
+961 1 74 44 61
;
_publ_contact_author_name
;
Kortz Ulrich
;
_publ_contact_author_phone
;
+961 3 77 64 39
;
_publ_section_title
;
Polyoxometalate-Diphosphate Complexes. 5.1 Cigar-Shaped
30-Molybdobispyrophosphate: Structure of
(N(C4H9)4)2H9[{(P2O7)Mo15O45}2][PMo12O40]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              623
_journal_page_last               624
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C138 Mo96 N12 O328 P11'
_chemical_formula_weight         16626.1
_space_group_IT_number           197
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I 2 2 3'
_symmetry_space_group_name_H-M   'I 2 3'
_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            4
_cell_length_a                   41.6910(4)
_cell_length_b                   41.6910(4)
_cell_length_c                   41.6910(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.81
_cell_measurement_theta_min      1.20
_cell_volume                     72464.8(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      173(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       '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  0.0958
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            212764
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         1.20
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.684
_exptl_absorpt_correction_T_max  0.744571
_exptl_absorpt_correction_T_min  0.561582
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details
;
2-theta dependent absorption corrections applied for an effective sphere
with mu*diameter = 0.400
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             30932
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.740
_refine_diff_density_min         -1.591
_refine_diff_density_rms         0.417
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(10)
_refine_ls_extinction_coef       1.68
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         12632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0848
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1359P)^2^+1956.2573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2415
_refine_ls_wR_factor_ref         0.2485
_reflns_number_gt                11954
_reflns_number_total             12632
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;

2021-08-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C46 Mo32 N4 O109.333 P3.667'
_cod_original_formula_weight         5541.41
_cod_original_formula_units_Z            12
_cod_database_code               4300074
_journal_paper_doi 10.1021/ic9907258