Three-dimensional bimetallic oxides constructed from molybdophosphonate chains and secondary-metal/4-pyridyltetrazole components
Stephanie Jones; Kari Darling; Jon Zubieta; Inorganica Chimica Acta 395 (2013) 89–94; doi:10.1016/j.ica.2012.10.022

data_1512892
_publ_section_title
;
 Three-dimensional bimetallic oxides constructed from molybdophosphonate
 chains and secondary-metal/4-pyridyltetrazole components
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              89
_journal_page_last               94
_journal_paper_doi               10.1016/j.ica.2012.10.022
_journal_volume                  395
_journal_year                    2013
_chemical_formula_moiety         'C42 H96 Mo15 N30 Ni6 O81 P6, 9(O)'
_chemical_formula_sum            'C42 H96 Mo15 N30 Ni6 O90 P6'
_chemical_formula_weight         4438.67
_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
_cell_angle_alpha                98.136(2)
_cell_angle_beta                 94.315(2)
_cell_angle_gamma                100.023(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3222(11)
_cell_length_b                   20.5941(17)
_cell_length_c                   22.4030(18)
_cell_measurement_reflns_used    1187
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.97
_cell_volume                     5960.2(8)
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_molecular_graphics    'CrystalMaker (Palmer,  2010)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX II CCD 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  0.0569
_diffrn_reflns_av_sigmaI/netI    0.1015
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            58827
_diffrn_reflns_theta_full        28.08
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    2.649
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4332
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.378
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1702
_refine_ls_number_reflns         28437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0646P)^2^+1.7196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1443
_reflns_number_gt                17935
_reflns_number_total             28437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-395-89-94-2.cif
_cod_data_source_block           p-1
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1512892