Pyro without Fire: Synthesis, Structure, and Reactivity of a Dimeric Vanadyl Pyrophosphate Coordination Complex
Nadia Marino; Susan K. Hanson; Peter Müller; Robert P. Doyle; Inorganic Chemistry 51 (2012) 10077–10079; doi:10.1021/ic3015767

data_4330517
_publ_section_title
;
 Pyro without Fire: Synthesis, Structure, and Reactivity of a Dimeric
 Vanadyl Pyrophosphate Coordination Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10077
_journal_page_last               10079
_journal_paper_doi               10.1021/ic3015767
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C20 H20 N4 O11 P2 V2, 3(H2 O)'
_chemical_formula_sum            'C20 H26 N4 O14 P2 V2'
_chemical_formula_weight         710.27
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.586(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0648(6)
_cell_length_b                   12.3888(7)
_cell_length_c                   20.0121(11)
_cell_measurement_reflns_used    5197
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      67.12
_cell_measurement_theta_min      4.53
_cell_volume                     2677.3(3)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2011)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2011)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2011)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL(Bruker,2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8048
_diffrn_reflns_theta_full        65.07
_diffrn_reflns_theta_max         65.07
_diffrn_reflns_theta_min         4.53
_exptl_absorpt_coefficient_mu    7.698
_exptl_absorpt_correction_T_max  0.9270
_exptl_absorpt_correction_T_min  0.6995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2287
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0531P)^2^+5.3451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                2156
_reflns_number_total             2287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3015767_si_002_1.cif
_cod_data_source_block           vpo22
_cod_database_code               4330517