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_1512893
_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         'C20 H24.50 Cu4 Mo5 N15 O23.75 P2'
_chemical_formula_sum            'C20 H24.5 Cu4 Mo5 N15 O23.75 P2'
_chemical_formula_weight         1650.83
_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                 114.353(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.662(3)
_cell_length_b                   15.9357(18)
_cell_length_c                   22.211(3)
_cell_measurement_reflns_used    9166
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.56
_cell_volume                     8274.8(18)
_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, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX 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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            40469
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    3.659
_exptl_absorpt_correction_T_max  0.5588
_exptl_absorpt_correction_T_min  0.2426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SHELXL-97 (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.647
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6348
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.276
_refine_diff_density_min         -2.131
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         10030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0283
_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^)+(0.1000P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1120
_reflns_number_gt                9264
_reflns_number_total             10030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-395-89-94-3.cif
_cod_data_source_block           c2c
_cod_original_cell_volume        8274.8(16)
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C20 H24.50 Cu4 Mo5 N15 O23.75 P2'
_cod_database_code               1512893