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_4311912
_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            'C108 H120.25 F4 Mo14 N24 Ni6 O78.25 P8'
_chemical_formula_weight         5025.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.7160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1269(7)
_cell_length_b                   36.9971(15)
_cell_length_c                   25.3324(10)
_cell_measurement_temperature    92(2)
_cell_volume                     15010.8(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            195733
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         1.37
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.058
_exptl_absorpt_correction_T_max  0.7903
_exptl_absorpt_correction_T_min  0.6836
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9897
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.670
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2198
_refine_ls_number_reflns         49909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+44.8893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                35367
_reflns_number_total             49909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049201ksi20040618_041150.cif
_cod_data_source_block           compound5
_cod_database_code               4311912