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_4311916
_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            'C49 H41 Mo7 N12 Ni2 O30.5 P2'
_chemical_formula_weight         2136.88
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 99.901(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8055(14)
_cell_length_b                   24.057(3)
_cell_length_c                   22.381(3)
_cell_measurement_reflns_used    864
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.16
_cell_measurement_theta_min      1.69
_cell_volume                     6261.6(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL and CrystalMaker 6.x'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'P4 w/ 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  0.0642
_diffrn_reflns_av_sigmaI/netI    0.1031
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34693
_diffrn_reflns_theta_full        29.16
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         1.69
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.001
_exptl_absorpt_coefficient_mu    2.094
_exptl_absorpt_correction_T_max  0.8504
_exptl_absorpt_correction_T_min  0.8179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             4172
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.495
_refine_diff_density_min         -1.228
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         16402
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                12863
_reflns_number_total             16402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049201ksi20040618_041245.cif
_cod_data_source_block           compound9
_cod_original_cell_volume        6261.5(13)
_cod_original_formula_sum        'C49 H41 Mo7 N12 Ni2 O30.50 P2'
_cod_database_code               4311916