Solid-State Coordination Chemistry of the Oxomolybdate-Organodiphosphonate/Nickel-Organoimine System: Structural Influences of the Secondary Metal Coordination Cation and Diphosphonate Tether Lengths
Eric Burkholder; Vladimir Golub; Charles J. O'Connor; Jon Zubieta; Inorganic Chemistry 43 (2004) 7014–7029; doi:10.1021/ic049201k

data_4311908
_publ_contact_author_address
;Department of Chemistry 
111 College Place
Syracuse University
Syracuse NY 13244    
;
_publ_contact_author_email       jazubiet@syr.edu
_publ_contact_author_fax         '(315) 443-4070'
_publ_contact_author_name        'Jon Zubieta'
_publ_contact_author_phone       '(315) 443-2547'
_publ_section_title
;
 Solid-State Coordination Chemistry of the
 Oxomolybdate-Organodiphosphonate/Nickel-Organoimine System: Structural
 Influences of the Secondary Metal Coordination Cation and Diphosphonate
 Tether Lengths
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7014
_journal_page_last               7029
_journal_paper_doi               10.1021/ic049201k
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C13 H12 Mo3 N3 Ni O15 P2'
_chemical_formula_weight         858.73
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.1350(10)
_cell_angle_beta                 75.4600(10)
_cell_angle_gamma                70.8870(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6676(5)
_cell_length_b                   11.0988(5)
_cell_length_c                   11.5999(6)
_cell_measurement_reflns_used    7126
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      1.89
_cell_volume                     1092.29(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL and CrystalMaker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'APEX CCD detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14236
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         1.89
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.001
_exptl_absorpt_coefficient_mu    2.764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             830
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         7126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0243P)^2^+1.1561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0580
_reflns_number_gt                6575
_reflns_number_total             7126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049201ksi20040618_041046.cif
_cod_data_source_block           compound1
_cod_database_code               4311908